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

HRID 1453012노트

반응식

HRID 1453012 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9bff387d10024f9591613e565833c3e8
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07473790B2

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