Реакция #1435739

Уравнение реакции

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

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title compound

Выход 92.0%

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

Выход 92.0%

Растворители

hydrochloric acid

Условия реакции

Обработка

1. 1
   ТемператураAfter cooling to 0° C. the reaction mixture
2. 2
   Промывкаwas washed twice with ether (50 ml)
3. 3
   workup.ADDITIONThe aqueous phase was treated with 50 ml dichloromethane
4. 4
   ДругоеThe organic phase was separated
5. 5
   Экстракцияthe aqueous phase was extracted four times with 50 ml dichloromethane
6. 6
   СушкаThe combined organic layers were dried over sodium sulfate
7. 7
   Концентрированиеconcentrated in vacuo

Методика

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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