Ethanol → 3-(4-Chlorobenzyl)-1-methyl-1H-pyrazol-5-ylamine

HRID 1808251노트

반응식

HRID 1808251 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=O)[CH2:10][C:11]#[N:12])=[CH:4][CH:3]=1.[CH3:14][NH:15][NH2:16].CCO>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]2[CH:10]=[C:11]([NH2:12])[N:15]([CH3:14])[N:16]=2)=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 6061MethylhydrazineHCID 509888474-(4-Chlorophenyl)-3-oxobutanenitrile

생성물 1

HCID 575512163-(4-Chlorobenzyl)-1-methyl-1H-pyrazol-5-ylamine수율 75%

실험 절차

A solution of 4-(4-chlorophenyl)-3-oxo-butyronitrile (Preparation 96, 2.2 g, 11 mmol) and N-methylhydrazine (1.94 mL, 36.5 mmol) in EtOH (40 mL, 800 mmol) was heated at 100° C. in a 40 mL vial (the reaction was split into 2 equal batches). After 20 h, the reaction mixture was cooled to rt and concentrated in vacuo. The residue was purified on the Isco (40 g SiO2, hexanes to ethyl acetate) to afford the title compound as an off-white solid (1.83 g, 69%).

후처리

  1. customwas split into 2 equal batches)
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified on the Isco (40 g SiO2, hexanes to ethyl acetate)

출처 및 근거

ORD 기록
ord-8081a1b37b8648ce847bdd7d9b56bfa0
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357711B2

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