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

HRID 3910

反応式

HRID 3910 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-49bd71cf48ae45fcbb90a9526cdec8dd
出典データセット
uspto-grants-1988_02
特許番号
US04723006

関連ノート

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