Triethylamine → 2-Chloro-N,N-dimethylpyrimidin-4-amine

HRID 1282168

反応式

HRID 1282168 の反応式
[CH3:1][NH:2][CH3:3].C(O)C.[Cl:7][C:8]1[N:13]=[C:12](Cl)[CH:11]=[CH:10][N:9]=1.C(N(CC)CC)C>O>[Cl:7][C:8]1[N:13]=[C:12]([N:2]([CH3:3])[CH3:1])[CH:11]=[CH:10][N:9]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 775312,4-DichloropyrimidineHCID 22184060Dimethylamine ethanol

生成物 1

HCID 959752-Chloro-N,N-dimethylpyrimidin-4-amine収率 59.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a 20% dimethylamine-ethanol solution (15.4 g) of 2,4-dichloropyrimidine (3.0 g) was added triethylamine (3 ml) under ice-cooling, and the mixture was stirred for 30 min. The reaction mixture was poured into water (100 ml) and extracted with ethyl acetate (100 ml). The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:hexane=1:1) to give the title compound (1.90 g) as white crystals, m.p.=77-79° C.

後処理

  1. temperaturecooling
  2. extractionextracted with ethyl acetate (100 ml)
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated
  6. customthe obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:hexane=1:1)

出典と根拠

ORDレコード
ord-a940852c62624a69ae773e7e9b6edebe
出典データセット
uspto-grants-2002_09
特許番号
US06455528B1

関連ノート

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