定制各类格氏试剂

问题:翻译一小段话
类型:求助 (悬赏分:3分)
提问:quick208
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版块:有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
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时间:2008-07-02 09:04:31  编辑    加入/取消收藏    订制/取消短消息    举报该贴    

Experimental
solution of MeNH, in methanol (5.4 mol dm 3, was obtained
y passing a stream of gaseous MeNH2, generated from 40%
queous MeNH2 and solid KOH, first through a drying tube
ith KOH pellets and then into the methanol at 0 "C. It was
andardized by acidimetric titration (HCl, Methyl Orange).
eagent quality solvents were used without further purification,
nd other reagents were used as supplied, by Aldrich Chemical
o., Merck Darmstadt Chemical Co. and Fluka Chemical Co.
agnesium (turnings for Grignard, 9939, was supplied by
erck. Melting points were taken with a Mel-Temp apparatus
nd are uncorrected. IR spectra were recorded with a Perkin-
lmer FT IR 1725X spectrometer, 'H NMR spectra with
ruker Spectrospin 600 MHz spectrometer and mass spectra
ith a Finnigan-Math instrument, model 8230. Gas chromato-
rams were obtained with a capillary Varian instrument, model
400, utilizing a capillary non-polar column, DB-5. The
actions were typically performed on a 50 mmol scale while
ome examples, like 3a, were also run on a 100, 150 and 200
mol scale with essentially the same yields. In general, on the
ale above, ca. 150 mmol, mechanical stirring was necessary.
ields refer to the pure oxalate salts unless otherwise stated,
nd were calculated to the corresponding amines when
arbonyl compounds were used in excess. Spectroscopic and
hysical data are given in Tables 1 and 2. Microanalytical data
r the new compounds are given in Table 3.
回复人:david_zhan,★★ () 时间:2008-07-03 18:33:24   编辑 1楼
仅供参考!
实验:
甲胺的甲醇溶液,(5.4 mol/dm 3,通过40%的甲胺和氢氧化钾发生,甲胺蒸汽通过氢氧化钾颗粒干燥管,然后由0度的甲醇溶液吸收制备),通过酸滴定进行标定(盐酸,甲基橙)。试剂级的溶剂使用前没有经过进一步的提纯,其他试剂使用Aldrich Chemical
o., Merck Darmstadt Chemical Co. and Fluka Chemical Co.
agnesium (turnings for Grignard, 9939, 等公司提供。熔点通过熔点仪测定,但是熔点仪没有经过校验,IR 光谱通过Perkin-
lmer FT IR 1725X 红外光谱仪测定,H NMR 核磁共振谱通过ruker Spectrospin 600 MHz 共振仪测定,质谱通过 Finnigan-Math instrument, model 8230质谱仪获得,气谱通过 Varian instrument, model
400毛细管气谱仪获得, 使用非极性DB-5毛细管柱获得。反应主要在50毫摩尔的规模进行,但也有一些反应象3a,是在100, 150 和 200毫摩尔的规模下进行,获得的收率相同,通常是在是在150毫摩尔, 机械搅拌式必需的。除非其他声明,收率是指纯残酸盐的收率,当羰基化合物过量时,收率是基于相应的胺计算的。 Spectroscopic and
hysical data are given in Tables 1 and 2. Microanalytical data
r the new compounds are given in Table 3.

[该帖子已被david_zhan在2008-07-03 22:00:28编辑过]


回复人:quick208, (以父之名) 时间:2008-07-04 13:36:52   编辑 2楼
已经打分了!

[该帖子已被david_zhan在2008-07-04 18:24:14编辑过]


得分人:david_zhan :3,


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