반응 #1435683

반응 방정식

2,4-diamino-6-methylanisole dihydrochloride

calcium carbonate

dioxane

2-chloroethyl chloroformate

→

Bis(2-chloroethyl) (4-methoxy-5-methyl-1,3-phenylene)biscarbamate

반응 조건

후처리

1. 1
   workup.WAITSubsequently, the mixture was left
2. 2
   온도to cool
3. 3
   여과the mineral salts were filtered off
4. 4
   workup.ADDITIONThe filtrate was poured onto iced water
5. 5
   추출the mixture was extracted several times with ethyl acetate
6. 6
   기타The combined ethyl acetate phases were then evaporated to dryness on a Rotavapor
7. 7
   기타giving pale brown crystals

실험 절차

56 g of 2,4-diamino-6-methylanisole dihydrochloride and 134 g of calcium carbonate were initially introduced into 1 l of dioxane and heated to 90° C. Within 15 min, 80 g of 2-chloroethyl chloroformate were added and the mixture was stirred for a further 4 h at this temperature. Subsequently, the mixture was left to cool, and the mineral salts were filtered off. The filtrate was poured onto iced water, and the mixture was extracted several times with ethyl acetate. The combined ethyl acetate phases were then evaporated to dryness on a Rotavapor, giving pale brown crystals.

출처