问题：求CAS:93-69-6 ,N-(2-Methylphenyl)imidodicarbonimidic diamide合成方法
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提问：flammable
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时间：2006-03-17 16:19:14 编辑加入/取消收藏订制/取消短消息举报该贴

CAS:93-69-6 英文名:O-Tolybiguanide 分子式:C9H13N5 分子量:191.23572
最好有文献.先谢谢!

[该帖子已被flammable在2006-3-20 22:21:29编辑过]

回复人：flammable,▲▲▲ (学无止境) 时间：2006-03-17 16:52:26 编辑

1楼

我现知道的资料:
Derivative: 1-N-(2-Methylphenyl)
Synonym(s): N-(2-Methylphenyl)imidodicarbonimidic diamide, 9CI
Chapman Hall Number: BOD26-D
CAS Registry Number: 93-69-6
Molecular Formula: C9H13N5
Molecular Weight: 191.235
Accurate Mass: 191.117095
Percentage Composition: C 56.53%; H 6.85%; N 36.62%
Use/Importance: Cross-linking agent for epoxy resins
Physical Description: Cryst. (H2O)
Melting Point: Mp 138. Mp 143-145
Aldrich: 42466-8

[该帖子已被flammable在2006-3-17 16:53:48编辑过]

回复人：flammable,▲▲▲ (学无止境) 时间：2006-03-17 16:54:14 编辑	2楼
请大家帮帮忙!

回复人：flammable,▲▲▲ (学无止境) 时间：2006-03-20 21:45:16 编辑	3楼
请有能之士帮下忙.

回复人：tangyyer,★★★★★ (有空来逛逛my blog: http://tangyyer.blog.hexun.com) 时间：2006-03-21 00:54:20 编辑

4楼

合成看看：FR 1461378；DD 61864。

The prepn. of the title compds. by treating an N1,N1-disubstituted biguanide with a diaralkyl phosphite in the presence of CCl4 and an alkali and catalytically hydrogenating the product. Thus, to 126 vols. pyrrolidine and 200 parts water, 135 vols. aq. HCl (d. 1.19) was added gradually, the mixt. was cooled to 30? and the water removed in vacuo The pyrrolidine-HCl was heated at 160?with 126 parts dicyandiamide for 2 hrs., the mixt. cooled to 60? 750 vols. MeOH added, the soln. filtered, and 875 vols. iso-Pr2O added carefully. After several days, the soln. was filtered, washed with MeOH-iso-Pr2O, and dried to give 140 parts tetramethylenebiguanide-HCl (I); picrate, m. 224? A mixt. of 52.4 parts dibenzyl phosphite in 185 vols. PhMe, 370 vols. CCl4, and 38.3 parts I in 115 vols. water was shaken vigorously and cooled to 2? 240 vols. 2.5N NaOH was added while the temp. was kept at 0-7? and the mixt. was shaken 6-7 hrs. and left overnight. CHCl3 (150 vols.) was added and decanted and the org. layer was washed with water contg. a little HOAc and distd. under reduced pressure. The residue was taken up in 150 vols. boiling EtOAc, filtered, combined with 270 vols. iso-Pr2O, filtered, washed with 1:1.8 EtOAc-iso-Pr2O, and dried to give 50 parts N5-dibenzyloxyphosphoryl-N1, N1-tetramethylenebiguanide (II), m. 107-8? II was hydrogenated in a mixt. of 16 parts II, 40 vols. 2N NaOH, 40 parts abs. EtOH, 18 parts 10% Pd-C, and H at a pressure slightly above atm. pressure until 1720 vols. H were absorbed and the soln. filtered, washed 3 times with 10 parts 50% EtOH, dild. with 300 parts dioxane, and left overnight. The soln. was filtered, washed, and dried to give 10 parts of the disodium salt of N5-phosphoryl-N1,N1-tetramethylenebiguanide.

The title compds. are prepd. from dicyandiamide (I) and arom. amines [esp. o-toluidine (II) or 2,5-xylidine (III)] in an aq. medium in the presence of HCl catalyst. HCl (4-7 wt.% less than the stoichiometric amt. based on arom. amines) is added to II or III, pH is held at 2-2.5, I (4-7 wt.% more than the stoichiometric amt. based on arom. amines) is added, the mixt. is heated to 365-369K and then cooled to 353-357K, and an aq. base soln. (4-7 wt.% more than the stoichiometric amt. necessary for neutralization of HCl) is added. The resulting crystals are sepd., washed, and dried. Thus, a mixt. of II 10.7, 30% HCl 12.2, and I 8 kg was heated at pH 2.3 and 365K, cooled during 4 h to 353K, mixed with 20% NaOH 44 kg, and cooled to 313K. The resulting crystals were sepd., rinsed with H2O, and dried at 353K to give 16.5 kg o-tolylbiguanide (contg. 0.3 wt.% NaCl).

回复人：flammable,▲▲▲ (学无止境) 时间：2006-03-24 20:49:37 编辑	5楼
已经打分了。

得分人：tangyyer-3,

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