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

HRID 1426362ノート

反応式

HRID 1426362 の反応式
[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

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 53404370HCID 53404370、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d06be6ba2b6a411889888009396e8f32
出典データセット
uspto-grants-2015_01
特許番号
US08933085B2

反応ノート

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