Реакция #4006

Уравнение реакции

dimethylamine hydrochloride

sodium

2-amino-4-chloro-6-chloromethylpyrimidine

→

2-amino-4-chloromethyl-6-dimethylaminopyrimidine

Растворители

methanol

methanol

Условия реакции

Обработка

1. 1
   workup.ADDITIONThe resulting mixture was added dropwise
2. 2
   ДругоеThe reaction was monitored by TLC and when reaction
3. 3
   Другоеwas evaporated
4. 4
   ДругоеThe solid obtained
5. 5
   Фильтрацияwas filtered
6. 6
   Другоеdried
7. 7
   ДругоеThe product was purified by chromatography on silica
8. 8
   Промывкаeluted with ethyl acetate
9. 9
   Другоеfollowed by sublimation at 110° C.

Методика

8.1 Parts of dimethylamine hydrochloride was added to a solution of 2.3 parts of sodium in 20 parts of methanol. The resulting mixture was added dropwise with stirring over about 10 minutes to a solution of 9.9 parts of 2-amino-4-chloro-6-chloromethylpyrimidine in 50 parts of methanol. The reaction was monitored by TLC and when reaction was complete the solvent was evaporated and the residue stirred with about 20 parts of water. The solid obtained was filtered and dried. The product was purified by chromatography on silica, eluted with ethyl acetate, followed by sublimation at 110° C./0.04 mb to give 2-amino-4-chloromethyl-6-dimethylaminopyrimidine m.p. 127°-129° C.

Источник