Sodium hydride → HCID 70922273, 화합물

HRID 524973노트

반응식

HRID 524973 반응식
[CH3:1][C:2]1[CH:6]=[CH:5][NH:4][C:3]=1[C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH3:16])=[O:8].[H-].[Na+].C1(C)C=C(C)C=C(C)C=1S(O[NH2:31])(=O)=O>CN(C=O)C>[NH2:31][N:4]1[CH:5]=[CH:6][C:2]([CH3:1])=[C:3]1[C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH3:16])=[O:8]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamineHCID 709222793-Methyl-N-o-tolyl-1H-pyrrole-2-carboxamide

생성물 1

HCID 70922273HCID 70922273, 화합물수율 73%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-Methyl-N-o-tolyl-1H-pyrrole-2-carboxamide (1.5 g, 7.00 mmol) was dissolved in 60 mL of DMF. 294 mg (7.35 mmol) of sodium hydride (60 wt % dispersion in mineral oil) were added and the reaction mixture was stirred at room temperature for 1 hour. Then O-(mesitylsulfonyl)hydroxylamine (1.658 g, 7.70 mmol) was added and the reaction mixture was stirred for 30 minutes. The solvent was evaporated to dryness and the crude product was purified by flash chromatography (0 to 50% heptane/AcOEt) to give 1.17 g (73% yield) of the title compound as a yellow solid.

후처리

  1. stirringthe reaction mixture was stirred for 30 minutes
  2. customThe solvent was evaporated to dryness
  3. customthe crude product was purified by flash chromatography (0 to 50% heptane/AcOEt)

출처 및 근거

ORD 기록
ord-c53a1c66857344e48c889215ec5a9ef5
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340547B2

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