反应 #5988

反应方程式

methyl chloroformate

1-methyl-5-(4-pyridinylamino)-1H-indole

→

solid

收率 98.4%

N-(1-Methyl-1H-indol-5-yl)-N-(4-pyridinyl) carbamic acid methyl ester

收率 98.4%

溶剂

DCM

DCM

triethylamine

反应条件

后处理

1. 1
   洗涤was washed with water and saturated sodium chloride
2. 2
   干燥dried (anhydrous magnesium sulfate)
3. 3
   过滤filtered
4. 4
   其他evaporated to 4 g of a solid
5. 5
   洗涤Elution through silica with 50% ethyl acetate in dichloromethane via flash column chromatography

实验过程

A solution of methyl chloroformate (1.3 g) in 5 ml DCM was added to a solution of 1-methyl-5-(4-pyridinylamino)-1H-indole (2.5 g) in 120 ml DCM and 6 ml triethylamine (4.4 g). After stirring one hour at ambient temperature the reaction mixture was washed with water and saturated sodium chloride, dried (anhydrous magnesium sulfate), filtered and evaporated to 4 g of a solid. Elution through silica with 50% ethyl acetate in dichloromethane via flash column chromatography yielded 3.1 g of a solid. Recrystallization from methanol yielded 2.4 g of crystals, mp 157°-159° C.

来源