Reacción #1435683

Ecuación de reacción

2,4-diamino-6-methylanisole dihydrochloride

calcium carbonate

dioxane

2-chloroethyl chloroformate

→

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

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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.

Fuente