Sodium borohydride → HCID 11372470, 화합물

HRID 644538노트

반응식

HRID 644538 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 11372470HCID 11372470, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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)+.

후처리

  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)+

출처 및 근거

ORD 기록
ord-239daf1ea2b144a9995990f6769d72fe
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700638B2

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