Dimethylamine, hydrochloride → 2-Amino-4-chloromethyl-6-dimethylaminopyrimidine

HRID 3910

반응식

HRID 3910 반응식
Cl.[CH3:2][NH:3][CH3:4].[Na].[NH2:6][C:7]1[N:12]=[C:11](Cl)[CH:10]=[C:9]([CH2:14][Cl:15])[N:8]=1>CO>[NH2:6][C:7]1[N:8]=[C:9]([CH2:14][Cl:15])[CH:10]=[C:11]([N:3]([CH3:4])[CH3:2])[N:12]=1

참가 물질

5

반응물 3

HCID 10473Dimethylamine, hydrochlorideHCID 5360545SodiumHCID 201534884-Chloro-6-(chloromethyl)pyrimidin-2-amine

생성물 1

HCID 201535022-Amino-4-chloromethyl-6-dimethylaminopyrimidine

시약·촉매·용매 1

HCID 887Methanol용매2회

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.

후처리

  1. additionThe resulting mixture was added dropwise
  2. customThe reaction was monitored by TLC and when reaction
  3. customwas evaporated
  4. customThe solid obtained
  5. filtrationwas filtered
  6. customdried
  7. customThe product was purified by chromatography on silica
  8. washeluted with ethyl acetate
  9. customfollowed by sublimation at 110° C.

출처 및 근거

ORD 기록
ord-49bd71cf48ae45fcbb90a9526cdec8dd
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04723006

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