Diisopropylethylamine → HCID 86755657, 화합물

HRID 1871992노트

반응식

HRID 1871992 반응식
[CH3:1][NH:2][CH2:3][C:4]([NH:6][C:7]1[S:8][CH:9]=[C:10]([CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:11]=1)=[O:5].C(N(CC)C(C)C)(C)C.F[C:28]1[N:33]=[C:32]([F:34])[CH:31]=[CH:30][N:29]=1>ClCCl>[F:34][C:32]1[CH:31]=[CH:30][N:29]=[C:28]([N:2]([CH3:1])[CH2:3][C:4]([NH:6][C:7]2[S:8][CH:9]=[C:10]([CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:11]=2)=[O:5])[N:33]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 1377162,4-DifluoropyrimidineHCID 86755656HCID 86755656, 화합물

생성물 1

HCID 86755657HCID 86755657, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The product of step (i) (3.0 g) was slurried in dichloromethane (100 ml) and treated with N,N-diisopropylethylamine (4.0 ml) forming a complete solution. 2,4-Difluoropyrimidine (J. Heterocyclic Chem. 1985, 22, 149) (0.6 g) was then added quickly with stirring. After 10 minutes the solvents were evaporated under reduced pressure and the residue purified by chromatography eluting with 20% ethyl acetate in isohexane. The first and minor component of the mixture to be eluted was the subtitle compound (0.77 g).

후처리

  1. customforming a complete solution
  2. customAfter 10 minutes the solvents were evaporated under reduced pressure
  3. customthe residue purified by chromatography
  4. washeluting with 20% ethyl acetate in isohexane
  5. washThe first and minor component of the mixture to be eluted

출처 및 근거

ORD 기록
ord-6fd795cb0a5e4022bb639d3e3545ef5a
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107297

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