Acetic Anhydride → 1-(4-Iodo-3,5-dimethyl-1H-pyrazol-1-yl)ethanone

HRID 1453012

反応式

HRID 1453012 の反応式
C(O[C:5](=[O:7])[CH3:6])(=O)C.C(N(CC)CC)C.[CH3:15][C:16]1[C:20]([I:21])=[C:19]([CH3:22])[NH:18][N:17]=1>C(Cl)Cl>[I:21][C:20]1[C:16]([CH3:15])=[N:17][N:18]([C:5](=[O:7])[CH3:6])[C:19]=1[CH3:22]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 971153,5-Dimethyl-4-iodo-1H-pyrazole

生成物 1

HCID 534715801-(4-Iodo-3,5-dimethyl-1H-pyrazol-1-yl)ethanone収率 85%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Acetic anhydride (0.51 mL, 5.4 mmol) and triethylamine (0.75 mL, 5.4 mmol) were added to a solution of 3,5-dimethyl-4-iodopyrazole (1 g, 4.5 mmol) in CH2Cl2. After 1 h the reaction mixture was partitioned between 1N HCl and EtOAc. The organic layer was washed with 1N HCl, saturated NaHCO3, brine, dried over Na2SO4, and concentrated to give the title compound as a white solid (1 g, 85%). 1H NMR (CDCl3): δ 2.27 (s, 3H), 2.60 (s, 3H), 2.66 (s, 3H).

後処理

  1. customAfter 1 h the reaction mixture was partitioned between 1N HCl and EtOAc
  2. washThe organic layer was washed with 1N HCl, saturated NaHCO3, brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-9bff387d10024f9591613e565833c3e8
出典データセット
uspto-grants-2009_01
特許番号
US07473790B2

関連ノート

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