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| CAS号 [5856-00-8] 生产工艺。 6’-氨基-N-乙基-N-苯甲酰基间甲苯胺 |
CAS号 [5856-00-8] 生产工艺。 6’-氨基-N-乙基-N-苯甲酰基间甲苯胺
CAS名：Benzamide, N-(4-amino-3-methylphenyl)-N-ethyl- 历史参考文献：待检索。
用途：有机合成。酸性蓝6。 LookChem网登录生产与经营单位26家。 反应类别：硝基还原。
BIOS 1153, 145-147.（=胶卷PB 85687）。 6’-Amino-N-ethylbenz-m-toluidide. (Leverkusen). 英国人译自德文（无资料来源）。
反应式：本人有加注，暂未找到德文原件。
Plant:
2000 l. C.I. reducer。 3000
l. C.I. extractor。 3000
l. wrought iron distillation pan。
3000
l. setting vessel。 Box
nutsche。 8000 l.
blow-egg。
Process:
The reducer is charged with 300 l. of water,
100 kg. of iron borings and 20 kg. of formic acid. 50 l. of toluene are added and the
nitro-compound is then charged in during 16 hours with simultaneous addition of
400 kg. of iron borings. Boiling with
indirect steam, is continued until reduction is complete (ca. 20 hours).
Test: A sample, worked up by extraction with
benzene, filtration and removal of solvent, must have a m.p. above 1000 and must give a clear solution in hydrochloric
acid.
The batch is then blown to the extractor and,
after addition of 20 kg. of soda ash and a little Terrana, is extracted with 7
lots of 1400 l. of benzene. The benzene
extracts are blown to the distillation vessel and the benzene recovered.
Towards the end of the benzene distillation,
some 500 l. of water are added and the remaining benzene removed by steam
distillation. The product precipitates
as fine pellets which are filtered on the nutsche. Yield = 90% theory. Quality: C. Pt. at least 990. 100 g ≈21-22 g. NaNO2 (Theory 100 = 27).
6”-Amino-N-ethylbenz-m-toluidide pure.
Plant: 1
Wooden or tile-lined vat (6000-8000 l.) with rubber covered steam pipe
and agitator。 1 Vat
6000-8000 l. with coil and cold water connections。
1 Nutsche 2-3 cu. m., wood or
tile-lined with filter tiles。 1 Tiled blow-egg, 6000-8000 l。
Charge: 6’-Amino-N-ethylbenz-m-toluidide
crude 575 kg. ≈150 kg. NaNO2。
Hydrochloric acid 19.50Be’ (30%)
250 l。
Carboraffin 25 kg。 Soda
ash (dissolved in water) 150 kg。
Process：
The wooden vat is charged with 3000 l. of
water at 80-900 and 250 l. of hydrochloric acid, and the 6’-amino-N-ethylbenz-m-toluidide
then charged. The product dissolves
easily in the dilute acid at 700 giving a violet colour on Congo paper. Only a trace of sludge remains which is
coagulated by addition of carbon (25 kg.) and sawdust (15 kg.).
The solution is run through the tiled nutsche
to the tiled blow-egg and the clear filtrate then blown into second vat. The base is precipitated by the slow addition
(5 hours) of a dilute sodium carbonate solution. At the end the solution should be still acid
to litmus: pH ca. 6. The product is
filtered and washed. Yield = 600 kg. moist
paste (100/23.75) = 143 kg. NaNO2 = 95% theory. C. Pt. = 102.4 – 1030.
张澍声 《精细化工中间体工业生产技术》1996年。 P. 56. 6-氨基-N-乙基-N-苯甲酰基间甲苯胺。 译自BIOS 1153, 143.
在2000 L还原釜中加入300 L水，100 kg铁屑和20 kg甲酸，再加入50 L甲苯。然后于16小时内加入硝基物，同时加入400 kg铁屑。用直接蒸汽煮沸，加完料后继续保持沸腾以完成还原（约20小时）。 检验：取样用苯萃取，过滤并除去溶剂，产品熔点应在100）C以上，在盐酸中应为清晰溶液。
将还原产物压入萃取器中，加入20 kg 碳酸钠和少量漂白土，用1400 L苯萃取7批，将苯萃取物压入蒸馏釜，蒸馏回收苯。蒸馏接近末期，加入500 L水，其余的苯用水蒸汽蒸馏除去，产品以小片状沉淀出来，抽滤，收率90%，熔点至少99℃。
6-氨基-N-乙基-N-苯甲酰基间甲苯胺纯品。
以下译文不再抄录，请读者谅解！
国内出版物：手头资料有限，未见有报导！
陈忠源 2019年1月29日星期二。（老有所乐，乐在其中！）。
文章作者：陈忠源 |
