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Lithium Hydroxide → HCID 66654755, 화합물

HRID 517709
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반응식

HRID 517709 반응식
C([O:4][CH2:5][C:6]1[N:10]([C:11]2[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[C:13]([C:19]([F:22])([F:21])[F:20])[CH:12]=2)[N:9]=[N:8][N:7]=1)(=O)C.[Li+].[OH-]>CCO.O>[OH:4][CH2:5][C:6]1[N:10]([C:11]2[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[C:13]([C:19]([F:22])([F:21])[F:20])[CH:12]=2)[N:9]=[N:8][N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 68074335{1-[4-cyano-3-(trifluoromethyl)phenyl]-1H-tetrazol-5-yl}methyl acetate

생성물 1

HCID 66654755HCID 66654755, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of 1-[4-cyano-3-(trifluoromethyl)phenyl]-1H-tetrazol-5-yl}methyl acetate (Intermediate 22, 45 g) in EtOH and water (2:1) was added LiOH (8.21 g, 0.342 mol) at 0° C. The reaction was stirred for 3 hours at room temperature. The solvent was removed under vacuum and the residue diluted with DCM, washed with ice-water, saturated aqueous NaHCO3 and brine. The solution was dried over anhydrous Na2SO4 and the solvent removed under vacuum. The crude product was purified by triturating with ether (500 mL) to yield 4-[5-(hydroxymethyl)-1H-tetrazol-1-yl]-2-(trifluoromethyl)benzonitrile as a viscous oil (30 g).

후처리

  1. customThe solvent was removed under vacuum
  2. additionthe residue diluted with DCM
  3. washwashed with ice-water, saturated aqueous NaHCO3 and brine
  4. dry with materialThe solution was dried over anhydrous Na2SO4
  5. customthe solvent removed under vacuum
  6. customThe crude product was purified
  7. customby triturating with ether (500 mL)

출처 및 근거

ORD 기록
ord-143ecc3896a94ab6aa3f10cbf6d8882f
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115132B2

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