Ammonium Acetate → 4-Methyl-6-(trifluoromethyl)pyridin-2(1H)-one

HRID 1426362노트

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HRID 1426362 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[O:5][C:4](=O)[CH:3]=1.C([O-])(=O)C.[NH4+:17]>C(O)(=O)C>[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[NH:17][C:4](=[O:5])[CH:3]=1

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 53404370HCID 53404370, 화합물

생성물 1

HCID 100351414-Methyl-6-(trifluoromethyl)pyridin-2(1H)-one

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
120 °C

실험 절차

To a solution of crude 4-methyl-6-(trifluoromethyl)-2H-pyran-2-one (28.8 g, 162 mmol) in acetic acid (330 mL) was added ammonium acetate (25.0 g, 324 mmol). The reaction solution was heated at 120° C. over weekend. The solvent was removed in vacuo. The residue was diluted with ethyl acetate and washed with saturated NaHCO3 and brine, dried over Na2SC4, filtered and concentrated. The crude was purified with pad silica gel. The solvent was removed. The solid was washed with 10:1 hexanes/ethyl acetate to give the desired product as white solid. LCMS (M+H)+: 178.0.

후처리

  1. customThe solvent was removed in vacuo
  2. additionThe residue was diluted with ethyl acetate
  3. washwashed with saturated NaHCO3 and brine
  4. dry with materialdried over Na2SC4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude was purified with pad silica gel
  8. customThe solvent was removed
  9. washThe solid was washed with 10:1 hexanes/ethyl acetate

출처 및 근거

ORD 기록
ord-d06be6ba2b6a411889888009396e8f32
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933085B2

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