4Iodo-benzoic acid N'-(2,2-dimethyl-propionyl)-hydrazide → 4-Iodobenzenecarbohydrazide

HRID 31410

반응식

HRID 31410 반응식
CC(C)(C)C([NH:5][NH:6][C:7](=[O:15])[C:8]1[CH:13]=[CH:12][C:11]([I:14])=[CH:10][CH:9]=1)=O>FC(F)(F)C(O)=O>[I:14][C:11]1[CH:12]=[CH:13][C:8]([C:7]([NH:6][NH2:5])=[O:15])=[CH:9][CH:10]=1

참가 물질

3

실험 절차

Trifluoroacetic acid (10 ml) was added to 4iodo-benzoic acid N′-(2,2-dimethyl-propionyl)-hydrazide (Intermediate 13) (1 g, 2.76 mmol) and stirred at room temperature for 2 hours. The trifluoroactic acid was removed in vacuo and the residue partitioned between ethyl acetate (50 ml) and saturated aqueous sodium bicarbonate solution (50 ml). The organic layer was washed with water (50 ml), brine (50 ml), dried over magnesium sulfate, filtered and the solvent removed in vacuo. The desired product was obtained as a white solid (0.55 g, 2.1 mmol).

후처리

  1. customThe trifluoroactic acid was removed in vacuo
  2. customthe residue partitioned between ethyl acetate (50 ml) and saturated aqueous sodium bicarbonate solution (50 ml)
  3. washThe organic layer was washed with water (50 ml), brine (50 ml)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-ac02ab09da504815b72b4796a3df3564
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425555B2

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