ethyl 3,3-bis(4-fluorophenyl)-2-(1-ethyl-1H-tetrazol-5-yl)-2-propenoate → 3,3-Bis(4-fluorophenyl)-2-(1-ethyl-1H-tetrazol-5-yl)-2-propenol

HRID 1195346노트

반응식

HRID 1195346 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)=[C:9]([C:15]2[N:19]([CH2:20][CH3:21])[N:18]=[N:17][N:16]=2)[C:10](OCC)=[O:11])=[CH:4][CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C>C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:22]2[CH:23]=[CH:24][C:25]([F:28])=[CH:26][CH:27]=2)=[C:9]([C:15]2[N:19]([CH2:20][CH3:21])[N:18]=[N:17][N:16]=2)[CH2:10][OH:11])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 14723820ethyl 3,3-bis(4-fluorophenyl)-2-(1-ethyl-1H-tetrazol-5-yl)-2-propenoateHCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 147238233,3-Bis(4-fluorophenyl)-2-(1-ethyl-1H-tetrazol-5-yl)-2-propenol수율 101.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of ethyl 3,3-bis(4-fluorophenyl)-2-(1-ethyl-1H-tetrazol-5-yl)-2-propenoate (1.0 g, 2.6 mmoles) at -78° in CH2Cl2 was rapidly added 7.8 mL (7.8 mmoles) of diisobutylaluminum hydride solution (1.0 Molar in methylene chloride). After stirring for 45 minutes, the mixture was quenched with 1N HCl solution. The organic layer was separated, dried (MgSO4) and concentrated in vacuo. The residual oil was triturated with hexane to give 0.9 g (100%) of the title compound; m.p.=103°-111° C.

후처리

  1. customat -78°
  2. customthe mixture was quenched with 1N HCl solution
  3. customThe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe residual oil was triturated with hexane

출처 및 근거

ORD 기록
ord-f3f913a4e17d48608e43b4b944c668a3
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05110940

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