تفاعل #1435739

معادلة التفاعل

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

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title compound

المردود 92.0%

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

المردود 92.0%

المذيبات

hydrochloric acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling to 0° C. the reaction mixture
2. 2
   غسيلwas washed twice with ether (50 ml)
3. 3
   workup.ADDITIONThe aqueous phase was treated with 50 ml dichloromethane
4. 4
   أخرىThe organic phase was separated
5. 5
   استخلاصthe aqueous phase was extracted four times with 50 ml dichloromethane
6. 6
   تجفيفThe combined organic layers were dried over sodium sulfate
7. 7
   تركيزconcentrated in vacuo

الإجراء التجريبي

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.

المصدر