反応 #1435683

反応方程式

2,4-diamino-6-methylanisole dihydrochloride

calcium carbonate

dioxane

2-chloroethyl chloroformate

→

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

反応条件

後処理

1. 1
   workup.WAITSubsequently, the mixture was left
2. 2
   温度to cool
3. 3
   ろ過the mineral salts were filtered off
4. 4
   workup.ADDITIONThe filtrate was poured onto iced water
5. 5
   抽出the mixture was extracted several times with ethyl acetate
6. 6
   その他The combined ethyl acetate phases were then evaporated to dryness on a Rotavapor
7. 7
   その他giving pale brown crystals

実験手順

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.

出典