Reaktion #4006

Reaktionsgleichung

dimethylamine hydrochloride

sodium

2-amino-4-chloro-6-chloromethylpyrimidine

→

2-amino-4-chloromethyl-6-dimethylaminopyrimidine

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONThe resulting mixture was added dropwise
2. 2
   SonstigeThe reaction was monitored by TLC and when reaction
3. 3
   Sonstigewas evaporated
4. 4
   SonstigeThe solid obtained
5. 5
   Filtrationwas filtered
6. 6
   Sonstigedried
7. 7
   SonstigeThe product was purified by chromatography on silica
8. 8
   Wascheneluted with ethyl acetate
9. 9
   Sonstigefollowed by sublimation at 110° C.

Vorschrift

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.

Quelle