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

HRID 1282168

반응식

HRID 1282168 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 775312,4-DichloropyrimidineHCID 22184060Dimethylamine ethanol

생성물 1

HCID 959752-Chloro-N,N-dimethylpyrimidin-4-amine수율 59.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-a940852c62624a69ae773e7e9b6edebe
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455528B1

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