Diisopropylethylamine → HCID 86755657、化合物

HRID 1871992ノート

反応式

HRID 1871992 の反応式
[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

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 1377162,4-DifluoropyrimidineHCID 86755656HCID 86755656、化合物

生成物 1

HCID 86755657HCID 86755657、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6fd795cb0a5e4022bb639d3e3545ef5a
出典データセット
uspto-grants-2000_08
特許番号
US06107297

反応ノート

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