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

HRID 239614

반응식

HRID 239614 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=7.1 Hz, 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-0765d842534943d4b4ec74ac697b09aa
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642607B2

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