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Ammonia → HCID 58656497, 화합물

HRID 1988935
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HRID 1988935 반응식
[CH:1]1([NH:4][C:5](=[O:22])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([C:13]3[CH:14]=[C:15]4[C:19](=[CH:20][CH:21]=3)[NH:18][N:17]=[CH:16]4)[CH:7]=2)[CH2:3][CH2:2]1.[H-].[Na+].Cl[CH2:26][C:27]([O:29][CH3:30])=[O:28].N>CN(C=O)C>[CH:1]1([NH:4][C:5]([C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([C:13]3[CH:14]=[C:15]4[C:19](=[CH:20][CH:21]=3)[N:18]([CH2:26][C:27]([O:29][CH3:30])=[O:28])[N:17]=[CH:16]4)[CH:7]=2)=[O:22])[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 7295Methyl chloroacetateHCID 24758Sodium hydrideHCID 10469531N-cyclopropyl-3-(1H-indazol-5-yl)-4-methylbenzamide

생성물 1

HCID 58656497HCID 58656497, 화합물수율 69.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of N-cyclopropyl-3-(1H-indazol-5-yl)-4-methylbenzamide (Example 17) (0.65 g) in dry DMF (26 ml) was treated with sodium hydride (60% oil dispersion, 0.134 g) under nitrogen. After 5 min methyl chloroacetate (0.29 g) was added and the mixture was stirred for 2 h. Aqueous ammonia (2M, 10 ml) was added and the solvent was removed under vacuum. The residue was purified by column chromatography on silica eluting with cyclohexane:ethyl acetate (2:1 to 1:1) to give the title compound (0.56 g).

후처리

  1. customthe solvent was removed under vacuum
  2. customThe residue was purified by column chromatography on silica eluting with cyclohexane:ethyl acetate (2:1 to 1:1)

출처 및 근거

ORD 기록
ord-c03e69e8fde64fb99923526affcd8867
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07642276B2

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