반응 #4378

반응 방정식

methylene chloride

oxalyl chloride

2-iodo-5-methoxybenzeneacetic acid

dimethylamine

→

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

용매

toluene

DMF

반응 조건

후처리

1. 1
   온도The solution was cooled to 0° C.
2. 2
   온도to warm to room temperature
3. 3
   workup.STIRRINGstir for three hours
4. 4
   세척The organic layer was washed with water, dilute hydrochloric acid, and sodium hydroxide
5. 5
   건조The organic layer was dried with MgSO4
6. 6
   기타evaporated in vacuo

실험 절차

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.

출처