Sodium hydride → HCID 70922273、化合物

HRID 524973ノート

反応式

HRID 524973 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 70922273HCID 70922273、化合物収率 73%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-c53a1c66857344e48c889215ec5a9ef5
出典データセット
uspto-grants-2016_05
特許番号
US09340547B2

反応ノート

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