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问题：请教各位大侠Dihydroxydibutylether的合成
类型：求助 (悬赏分:3分)
提问：bene
等级：▲▲
版块：有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
信誉：100%
回复：15
阅读：2162
时间：2005-08-02 18:11:17  编辑    加入/取消收藏    订制/取消短消息    举报该贴    

Dihydroxydibutylether（丁醚二醇）如何合成？
回复人：yfqycxlele,▲ (从事药物合成，药品注册，及报批资料整理等工作) 时间：2006-07-05 11:40:33   编辑 1楼
对不起，我目前正查询有关其合成的资料或文献，谁有能贡献一下吗？先谢啦！


回复人：bene,▲▲ (药物合成初学者) 时间：2006-07-28 18:15:46   编辑 2楼
已经打分了。


回复人：tomao,▲ (我是一名药物合成爱好者！) 时间：2006-08-01 16:39:38   编辑 3楼
正在找呢！


回复人：tomao,▲ (我是一名药物合成爱好者！) 时间：2006-08-01 16:41:55   编辑 4楼
去哪里找合成文献呢！
可参考！
Monograph Number: 7029
Title: 4,4¢-Oxydi-2-butanol
CAS Registry Number: 821-33-0
CAS Name: 4,4¢-Oxybis[2-butanol]
Additional Names: 3,3¢-dihydroxydibutyl ether; bis[3-hydroxybutyl] ether; DHBE
Trademarks: Diskin; Dyskinébyl (Saunier); Dis-Cinil (Lusofarmaco); Colenormol
Molecular Formula: C8H18O3
Molecular Weight: 162.23.
Percent Composition: C 59.23%, H 11.18%, O 29.59%
Line Formula: CH3CH(OH)CH2CH2OCH2CH2CH(OH)CH3
Literature References: Prepn: Joulty, FR 1267084 (1960). Action on bile flow: Bornmann, Arzneimittel-Forsch. 2, 122 (1952). Use as choleretic and antispasmodic: Albot, Toulet, Presse Med. 67, 2053 (1959). General pharmacological properties: Fregnan, Porta, Arzneimittel-Forsch. 26, 2116 (1976).
Properties: Clear, almost colorless, bitter fluid. Miscible with water.
Therap-Cat: Choleretic.


回复人：eeehcl,▲ () 时间：2006-09-14 21:33:07   编辑 5楼
请问bene，Dihydroxydibutylether的合成问题解决了吗？该产品是单一化合物吗？我用GC检法国纳化市售品出了3个峰。


回复人：bene,▲▲ (药物合成初学者) 时间：2006-09-22 14:47:01   编辑 6楼
老兄,正在做呢,产品肯定是单一化合物,是不是你所购的纯度不够,其它两个是什么?做了吗?


回复人：qyl1970,★ (专注于有机合成，接受公斤级化合物定制。) 时间：2005-08-02 19:55:37   编辑 7楼
丁二醇控制下醚化即可。


回复人：zxl_mumu,▲ (一无是处) 时间：2005-08-02 21:13:54   编辑 8楼
丁二醇醚化



回复人：bene,▲▲ (药物合成初学者) 时间：2005-08-03 18:25:46   编辑 9楼
如何控制？


回复人：lshr2003,▲ (学习无止静，活到老，学到老，希望大学多多指导) 时间：2007-09-05 17:23:23   编辑 10楼
我查到一篇文献，大家分享：
High molecular polyether carboxylic acids, containing at least two ether oxygen atoms and not more than three alkyleneoxy groups directly connected together are prepared by introducing at least one carboxylic group, by the following methods, into polyethers derived from aliphatic polyhydric alcohols having from 2-4 carbon atoms and containing at least one aliphatic, cycloaliphatic or mixed aromaticaliphatic radicle having at least 8 carbon atoms attached to the ether radicle by means of oxygen, nitrogen or sulphur: (a) when the polyethers contain a mineral acid residue they are treated with hydrocyanic acid or its salts and the resulting nitriles saponified; (b) when the polyethers contain a terminal CH2OH group, they are oxidized to the corresponding carboxylic acid or are converted into the alkali alcoholate and condensed with low molecular halogen carboxylic acids or are esterified with polycarboxylic acids to give ester-acids; (c) when the polyethers contain an amino group they are reacted with a mineral acid ester of a hydroxycarboxylic acid or a polycarboxylic acid. The same products are obtained by treating polyether carboxylic acids which contain hydroxy or amino groups with high molecular carboxylic acids or their halides, alcohols of high molecular weight or alkylated phenols, and also by treating polyether dicarboxylic acids with amines or alcohols of high molecular weight. The products are stated to be wetting, washing, softening, foaming and emulsifying agents. In examples: (1) sodium monochloracetate is condensed with sodium dodecyltriethyleneglycolether and with the sodium compound of a polyhydroxyethylated octodecylalcohol; (2) bis-ethyleneglycollic acid anhydride is reacted with dodecyl alcohol and with oleylamine; (3) dodecyl triethyleneglycolether is oxidized to the carboxylic acid with nitric acid; (4) oleic acid chloride is condensed with the substituted glycocoll obtained from the sulphuric ester of diethyleneglycolmonoethylether and glycocoll; (5) octodecyltriethyleneglycolchlormethylether, obtained from hydrochloric acid, trioxymethylene and octodecyltriethyleneglycol, is treated with cuprous cyanide and the nitrile saponified; (6) phthalic anhydride is reacted with (a) diethyleneglycolmono dodecyl, octodecenyl or naphthenyl ether, (b) the acid amide obtained by condensing hardened train oil fatty acids with ethanolamine and treating with ethylene oxide and (c) the amine obtained by condensing methylamine with the sulphuric ester of diethylene glycolmonododecylether. Maleic, chlormaleic, succinic, adipic, diglycollic, thiodiglycollic and oxalic acids are specified polycarboxylic acids which may be used. Diethyleneglycol - b dodecylether - b <1> - N - methylaminoacetic acid, diethyleneglycol - b - octodecylether - b <1> - N - benzylaminomaleicmonoamide and diethyleneglycol -b - octadecenylether - b <1> - phthalic acid monoester are products which are mentioned. Samples have been furnished under Sect. 2 (5) as follows: (1) phthalic acid monoester of iso


回复人：lshr2003,▲ (学习无止静，活到老，学到老，希望大学多多指导) 时间：2007-09-05 17:24:13   编辑 11楼
我查到一篇文献，大家分享：
High molecular polyether carboxylic acids, containing at least two ether oxygen atoms and not more than three alkyleneoxy groups directly connected together are prepared by introducing at least one carboxylic group, by the following methods, into polyethers derived from aliphatic polyhydric alcohols having from 2-4 carbon atoms and containing at least one aliphatic, cycloaliphatic or mixed aromaticaliphatic radicle having at least 8 carbon atoms attached to the ether radicle by means of oxygen, nitrogen or sulphur: (a) when the polyethers contain a mineral acid residue they are treated with hydrocyanic acid or its salts and the resulting nitriles saponified; (b) when the polyethers contain a terminal CH2OH group, they are oxidized to the corresponding carboxylic acid or are converted into the alkali alcoholate and condensed with low molecular halogen carboxylic acids or are esterified with polycarboxylic acids to give ester-acids; (c) when the polyethers contain an amino group they are reacted with a mineral acid ester of a hydroxycarboxylic acid or a polycarboxylic acid. The same products are obtained by treating polyether carboxylic acids which contain hydroxy or amino groups with high molecular carboxylic acids or their halides, alcohols of high molecular weight or alkylated phenols, and also by treating polyether dicarboxylic acids with amines or alcohols of high molecular weight. The products are stated to be wetting, washing, softening, foaming and emulsifying agents. In examples: (1) sodium monochloracetate is condensed with sodium dodecyltriethyleneglycolether and with the sodium compound of a polyhydroxyethylated octodecylalcohol; (2) bis-ethyleneglycollic acid anhydride is reacted with dodecyl alcohol and with oleylamine; (3) dodecyl triethyleneglycolether is oxidized to the carboxylic acid with nitric acid; (4) oleic acid chloride is condensed with the substituted glycocoll obtained from the sulphuric ester of diethyleneglycolmonoethylether and glycocoll; (5) octodecyltriethyleneglycolchlormethylether, obtained from hydrochloric acid, trioxymethylene and octodecyltriethyleneglycol, is treated with cuprous cyanide and the nitrile saponified; (6) phthalic anhydride is reacted with (a) diethyleneglycolmono dodecyl, octodecenyl or naphthenyl ether, (b) the acid amide obtained by condensing hardened train oil fatty acids with ethanolamine and treating with ethylene oxide and (c) the amine obtained by condensing methylamine with the sulphuric ester of diethylene glycolmonododecylether. Maleic, chlormaleic, succinic, adipic, diglycollic, thiodiglycollic and oxalic acids are specified polycarboxylic acids which may be used. Diethyleneglycol - b dodecylether - b <1> - N - methylaminoacetic acid, diethyleneglycol - b - octodecylether - b <1> - N - benzylaminomaleicmonoamide and diethyleneglycol -b - octadecenylether - b <1> - phthalic acid monoester are products which are mentioned. Samples have been furnished under Sect. 2 (5) as follows: (1) phthalic acid monoester of iso


回复人：lshr2003,▲ (学习无止静，活到老，学到老，希望大学多多指导) 时间：2007-09-05 17:24:14   编辑 12楼
我查到一篇文献，大家分享：
High molecular polyether carboxylic acids, containing at least two ether oxygen atoms and not more than three alkyleneoxy groups directly connected together are prepared by introducing at least one carboxylic group, by the following methods, into polyethers derived from aliphatic polyhydric alcohols having from 2-4 carbon atoms and containing at least one aliphatic, cycloaliphatic or mixed aromaticaliphatic radicle having at least 8 carbon atoms attached to the ether radicle by means of oxygen, nitrogen or sulphur: (a) when the polyethers contain a mineral acid residue they are treated with hydrocyanic acid or its salts and the resulting nitriles saponified; (b) when the polyethers contain a terminal CH2OH group, they are oxidized to the corresponding carboxylic acid or are converted into the alkali alcoholate and condensed with low molecular halogen carboxylic acids or are esterified with polycarboxylic acids to give ester-acids; (c) when the polyethers contain an amino group they are reacted with a mineral acid ester of a hydroxycarboxylic acid or a polycarboxylic acid. The same products are obtained by treating polyether carboxylic acids which contain hydroxy or amino groups with high molecular carboxylic acids or their halides, alcohols of high molecular weight or alkylated phenols, and also by treating polyether dicarboxylic acids with amines or alcohols of high molecular weight. The products are stated to be wetting, washing, softening, foaming and emulsifying agents. In examples: (1) sodium monochloracetate is condensed with sodium dodecyltriethyleneglycolether and with the sodium compound of a polyhydroxyethylated octodecylalcohol; (2) bis-ethyleneglycollic acid anhydride is reacted with dodecyl alcohol and with oleylamine; (3) dodecyl triethyleneglycolether is oxidized to the carboxylic acid with nitric acid; (4) oleic acid chloride is condensed with the substituted glycocoll obtained from the sulphuric ester of diethyleneglycolmonoethylether and glycocoll; (5) octodecyltriethyleneglycolchlormethylether, obtained from hydrochloric acid, trioxymethylene and octodecyltriethyleneglycol, is treated with cuprous cyanide and the nitrile saponified; (6) phthalic anhydride is reacted with (a) diethyleneglycolmono dodecyl, octodecenyl or naphthenyl ether, (b) the acid amide obtained by condensing hardened train oil fatty acids with ethanolamine and treating with ethylene oxide and (c) the amine obtained by condensing methylamine with the sulphuric ester of diethylene glycolmonododecylether. Maleic, chlormaleic, succinic, adipic, diglycollic, thiodiglycollic and oxalic acids are specified polycarboxylic acids which may be used. Diethyleneglycol - b dodecylether - b <1> - N - methylaminoacetic acid, diethyleneglycol - b - octodecylether - b <1> - N - benzylaminomaleicmonoamide and diethyleneglycol -b - octadecenylether - b <1> - phthalic acid monoester are products which are mentioned. Samples have been furnished under Sect. 2 (5) as follows: (1) phthalic acid monoester of iso


回复人：大龙随缘,▲ (化学有机合成，原料药) 时间：2010-12-23 15:38:25   编辑 13楼
可以把dihydroxydibutylether的文献发我邮箱吗？急需，拜托诸位大神了，


回复人：大龙随缘,▲ (化学有机合成，原料药) 时间：2010-12-23 15:41:08   编辑 14楼
可以把dihydroxydibutylether的文献发我邮箱吗？急需，拜托诸位大神了，我的邮箱lanyanlonger@163.com


回复人：大龙随缘,▲ (化学有机合成，原料药) 时间：2011-02-11 07:39:24   编辑 15楼
为什么没人啊！


得分人：zxl_mumu-1,

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