反应 #4378

反应方程式

methylene chloride

oxalyl chloride

2-iodo-5-methoxybenzeneacetic acid

dimethylamine

→

N,N-dimethyl-2-iodo-5-methoxybenzeneacetamide

溶剂

toluene

DMF

反应条件

后处理

1. 1
   温度The solution was cooled to 0° C.
2. 2
   温度to warm to room temperature
3. 3
   workup.STIRRINGstir for three hours
4. 4
   洗涤The organic layer was washed with water, dilute hydrochloric acid, and sodium hydroxide
5. 5
   干燥The organic layer was dried with MgSO4
6. 6
   其他evaporated in vacuo

实验过程

A 16.7 g (0.19 mole) sample of oxalyl chloride was added dropwise at 0° C. to a solution of 50.0 g (0.17 mole) of 2-iodo-5-methoxybenzeneacetic acid in 310 ml dry toluene and 31.7 ml of DMF. The mixture was allowed to warm to room temperature and stir for 16 hours. The solution was cooled to 0° C. and dimethylamine gas was admitted until the mixture was strongly basic. The mixture was allowed to warm to room temperature and stir for three hours and methylene chloride was added. The organic layer was washed with water, dilute hydrochloric acid, and sodium hydroxide. The organic layer was dried with MgSO4 and evaporated in vacuo to give 54.2 g of N,N-dimethyl-2-iodo-5-methoxybenzeneacetamide, mp 86°-89° C.

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