反応 #5988

反応方程式

methyl chloroformate

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

→

solid

収率 98.4%

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

収率 98.4%

溶媒

DCM

DCM

triethylamine

反応条件

後処理

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

実験手順

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.

出典