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Sodium hydride → HCID 121386233, 화합물

HRID 2203015
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HRID 2203015 반응식
[Br:1][C:2]1[N:3]=[CH:4][C:5]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[N:6][CH:7]=1.[H-].[Na+].Br[CH:22]([CH3:28])[C:23]([CH:25]1[CH2:27][CH2:26]1)=[O:24]>CN(C=O)C>[Br:1][C:2]1[N:3]=[CH:4][C:5](=[N:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])[N:6]([CH:22]([CH3:28])[C:23]([CH:25]2[CH2:27][CH2:26]2)=[O:24])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 450808052-Bromo-1-cyclopropylpropan-1-oneHCID 57749444HCID 57749444, 화합물

생성물 1

HCID 121386233HCID 121386233, 화합물수율 45.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of N-(5-bromopyrazin-2-yl)-4-methylbenzenesulfonamide (1.73 g) in DMF (20 ml) was added NaH (60% in oil, 0.316 g) at 0° C., and the mixture was stirred at room temperature for 30 min. To the mixture was added 2-bromo-1-cyclopropylpropan-1-one (1.87 g) at room temperature, and the mixture was stirred overnight. The mixture was partitioned between EtOAc and water, and the organic layer was washed with brine, dried over MgSO4, concentrated in vacuo, and purified by silica gel column chromatography (hexane/EtOAc) to give the title compound (1.02 g) as a solid.

후처리

  1. stirringthe mixture was stirred overnight
  2. customThe mixture was partitioned between EtOAc and water
  3. washthe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. custompurified by silica gel column chromatography (hexane/EtOAc)

출처 및 근거

ORD 기록
ord-90018ebbe19c46ebba75d64ac018ace1
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365540B2

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