1,2-Dichloroethane → HCID 47149234、化合物

HRID 216330ノート

反応式

HRID 216330 の反応式
[CH3:1][NH:2][O:3][CH3:4].[N:5]1([C:10]2[CH:18]=[CH:17][C:13]([C:14]([OH:16])=O)=[CH:12][N:11]=2)[CH:9]=[CH:8][CH:7]=[N:6]1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.CN1CCOCC1>C(Cl)Cl>[CH3:4][O:3][N:2]([CH3:1])[C:14](=[O:16])[C:13]1[CH:17]=[CH:18][C:10]([N:5]2[CH:9]=[CH:8][CH:7]=[N:6]2)=[N:11][CH:12]=1

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 14232N,O-DimethylhydroxylamineHCID 757711-HydroxybenzotriazoleHCID 27636146-(1H-pyrazol-1-yl)nicotinic acid

生成物 1

HCID 47149234HCID 47149234、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

N,O-Dimethylhydroxylamine (1.03 g, 10.6 mmol) was added to an ambient temperature solution of 6-(1H-pyrazol-1-yl)nicotinic acid (2 g, 10.6 mmol), EDC (2.4 g, 12.7 mmol), HOBt (1.94 g, 12.7 mmol) and NMM (5.2 mL, 47.6 mmol) in methylene chloride (100 mL). After stirring at ambient temperature overnight, the reaction mixture was diluted with methylene chloride and washed successively with saturated aqueous sodium bicarbonate and brine, dried (sodium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-100% ethyl acetate/hexane afforded N-methoxy-N-methyl-6-(1H-pyrazol-1-yl)nicotinamide.

後処理

  1. washwashed successively with saturated aqueous sodium bicarbonate and brine
  2. dry with materialdried (sodium sulfate)
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2750ff61d60b45698c90dddaa4e38ddc
出典データセット
uspto-grants-2012_06
特許番号
US08193228B2

反応ノート

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