1,2-Dichloroethane → HCID 47149234, 화합물

HRID 216330노트

반응식

HRID 216330 반응식
[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

참가 물질

7

반응물 5

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

생성물 1

HCID 47149234HCID 47149234, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2750ff61d60b45698c90dddaa4e38ddc
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193228B2

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