反应 #1435739

反应方程式

N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-2,2-dimethyl-propionamide

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title compound

收率 92.0%

4-Iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-ylamine

收率 92.0%

溶剂

hydrochloric acid

反应条件

后处理

1. 1
   温度After cooling to 0° C. the reaction mixture
2. 2
   洗涤was washed twice with ether (50 ml)
3. 3
   workup.ADDITIONThe aqueous phase was treated with 50 ml dichloromethane
4. 4
   其他The organic phase was separated
5. 5
   萃取the aqueous phase was extracted four times with 50 ml dichloromethane
6. 6
   干燥The combined organic layers were dried over sodium sulfate
7. 7
   浓缩concentrated in vacuo

实验过程

A mixture of 2.20 g (5.47 mmol) N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-2,2-dimethyl-propionamide (synthesis described in DE10008042) in 50 ml 3 N hydrochloric acid was stirred for 18 h at 100° C. After cooling to 0° C. the reaction mixture was washed twice with ether (50 ml). The aqueous phase was treated with 50 ml dichloromethane and basified with a 1 M solution of sodium carbonate. The organic phase was separated and the aqueous phase was extracted four times with 50 ml dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 1.60 g (92%) of the title compound as an off-white solid.

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