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Sodium hydride → HCID 58042316, 화합물

HRID 1619689
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HRID 1619689 반응식
[H-].[Na+].[Br:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([C:11]2[N:15]([CH3:16])[N:14]=[CH:13][CH:12]=2)[CH:5]=1.[C:17]([C:19]1[CH:20]=[C:21]([S:26]([N:29]([CH2:35][C:36]2[CH:41]=[CH:40][C:39]([O:42][CH3:43])=[CH:38][C:37]=2[O:44][CH3:45])[C:30]2[S:31][CH:32]=[CH:33][N:34]=2)(=[O:28])=[O:27])[CH:22]=[CH:23][C:24]=1F)#[N:18]>CN(C=O)C.C(OCC)(=O)C>[Br:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][C:24]2[CH:23]=[CH:22][C:21]([S:26]([N:29]([CH2:35][C:36]3[CH:41]=[CH:40][C:39]([O:42][CH3:43])=[CH:38][C:37]=3[O:44][CH3:45])[C:30]3[S:31][CH:32]=[CH:33][N:34]=3)(=[O:28])=[O:27])=[CH:20][C:19]=2[C:17]#[N:18])=[C:6]([C:11]2[N:15]([CH3:16])[N:14]=[CH:13][CH:12]=2)[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 58042307HCID 58042307, 화합물HCID 136200892HCID 136200892, 화합물

생성물 1

HCID 58042316HCID 58042316, 화합물수율 87.1%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate
용매

실험 절차

To a slurry of sodium hydride (54 mg, 1.4 mmol, 60% in mineral oil) in DMF (1 mL) was added 4-bromo-2-(1-methyl-1H-pyrazol-5-yl)phenol (Preparation 89, 210 mg, 0.83 mmol) as a solution in DMF (3 mL). After stirring for 30 minutes, 3-cyano-N-(2,4-dimethoxy-benzyl)-4-fluoro-N-thiazol-2-yl-benzenesulfonamide (Preparation 90, 415 mg, 0.957 mmol) was added. After 3 hours the reaction mixture was diluted with ethyl acetate (10 mL) and washed with water (5 mL) and brine (5 mL). The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. Purification by automated flash column chromatography using a 0-100% ethyl acetate/dichloromethane gradient provided the title compound (482 mg, 87%) as a yellow foam.

후처리

  1. washwashed with water (5 mL) and brine (5 mL)
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customPurification by automated flash column chromatography

출처 및 근거

ORD 기록
ord-9ef65792672c49e4bb8a3d28c0d057d0
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772293B2

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