Sodium Acetate → 6-Methoxy-2-methyl-3-phenyl-4H-chromen-4-one

HRID 1476154

반응식

HRID 1476154 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10](=[O:18])[CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[C:19]([O-])(=O)[CH3:20].[Na+]>C(OC(=O)C)(=O)C>[CH3:9][O:8][C:5]1[CH:4]=[C:3]2[C:2](=[CH:7][CH:6]=1)[O:1][C:19]([CH3:20])=[C:11]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:10]2=[O:18]

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 27756071-(2-Hydroxy-5-methoxyphenyl)-2-phenylethanone

생성물 1

HCID 665791676-Methoxy-2-methyl-3-phenyl-4H-chromen-4-one수율 68.2%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

Intermediate 20 (4 g, 16.51 mmoles) was taken in a RB flask and to this acetic anhydride (40 ml) and sodium acetate (9.48 g, 115.57 mmoles) were added and the mixture was refluxed for 12 h. After cooling to RT, the reaction mixture was quenched by the addition of ice cold water. The solid formed was filtered and washed with water. The product was dried under vacuum to afford the title compound as yellow solid (3 g, 68% yield). 1H-NMR (δ ppm, CDCl3, 400 MHz): δ 7.60(d, J=3.0 Hz, 1H), 7.45(t, J=7.1Hz, 2H), 7.37(m, 2H), 7.29(m, 3H), 3.89(s, 3H).2.31(s, 3H).

후처리

  1. additionwere added
  2. temperaturethe mixture was refluxed for 12 h
  3. customthe reaction mixture was quenched by the addition of ice cold water
  4. customThe solid formed
  5. filtrationwas filtered
  6. washwashed with water
  7. customThe product was dried under vacuum

출처 및 근거

ORD 기록
ord-52a6bc4ababc44e8b5e63803e9303919
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018375B2

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