Sodium borohydride → HCID 11372470、化合物

HRID 644538ノート

反応式

HRID 644538 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([C:10]2[C:15]3[N:16]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:17]=[N:18][C:14]=3[CH:13]=[C:12]([C:25]([F:28])([F:27])[F:26])[CH:11]=2)[CH:7]=[CH:8][CH:9]=1)(=[O:3])[CH3:2].[BH4-].[Na+]>C(O)C>[OH:3][CH:1]([C:4]1[CH:5]=[C:6]([C:10]2[C:15]3[N:16]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:17]=[N:18][C:14]=3[CH:13]=[C:12]([C:25]([F:28])([F:27])[F:26])[CH:11]=2)[CH:7]=[CH:8][CH:9]=1)[CH3:2]

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 114289357-(3-Acetylphenyl)-1-phenyl-5-trifluoromethylbenzimidazole

生成物 1

HCID 11372470HCID 11372470、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 7-(3-acetylphenyl)-1-phenyl-5-trifluoromethylbenzimidazole (0.95 g, 2.5 mmol) in ethanol (10 ml) was added sodium borohydride (0.1 g, 2.6 mmol) and the resultant mixture was stirred at 60° C. for 20 min. The cooled reaction mixture was concentrated under reduced pressure and the concentrate was partitioned between ethyl acetate and water. The organic layer was dried over magnesium sulphate and concentrated to a small volume (1-2 ml) under reduced pressure. The title product precipitated upon addition of ligroin to the concentrate (0.65 g, 68%) m/z, 383.1 (M+H)+.

後処理

  1. customThe cooled reaction mixture
  2. concentrationwas concentrated under reduced pressure
  3. customthe concentrate was partitioned between ethyl acetate and water
  4. dry with materialThe organic layer was dried over magnesium sulphate
  5. concentrationconcentrated to a small volume (1-2 ml) under reduced pressure
  6. customThe title product precipitated upon addition of ligroin to the
  7. concentrationconcentrate (0.65 g, 68%) m/z, 383.1 (M+H)+

出典と根拠

ORDレコード
ord-239daf1ea2b144a9995990f6769d72fe
出典データセット
uspto-grants-2010_04
特許番号
US07700638B2

反応ノート

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