반응 #4006

반응 방정식

dimethylamine hydrochloride

sodium

2-amino-4-chloro-6-chloromethylpyrimidine

→

2-amino-4-chloromethyl-6-dimethylaminopyrimidine

용매

methanol

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONThe resulting mixture was added dropwise
2. 2
   기타The reaction was monitored by TLC and when reaction
3. 3
   기타was evaporated
4. 4
   기타The solid obtained
5. 5
   여과was filtered
6. 6
   기타dried
7. 7
   기타The product was purified by chromatography on silica
8. 8
   세척eluted with ethyl acetate
9. 9
   기타followed by sublimation at 110° C.

실험 절차

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.

출처