Pyridine → 2,3-Dihydro-1-oxo-3-phenyl-1H-inden-6-yl acetate

HRID 331261노트

반응식

HRID 331261 반응식
[OH:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:7][C:8]2=[O:11])=[CH:4][CH:3]=1.N1C=CC=CC=1.[C:24](OC(=O)C)(=[O:26])[CH3:25]>C(Cl)Cl.CCOC(C)=O>[C:24]([O:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]([C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:7][C:8]2=[O:11])=[CH:4][CH:3]=1)(=[O:26])[CH3:25]

참가 물질

6

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 703075012,3-Dihydro-6-hydroxy-3-phenylinden-1-one

생성물 1

HCID 703172342,3-Dihydro-1-oxo-3-phenyl-1H-inden-6-yl acetate수율 77%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

2,3-Dihydro-6-hydroxy-3-phenylinden-1-one (22.5 g, 100 mmol) obtained in Step 2 was placed into a flask and dissolved in CH2Cl2 (300 mL). To the solution at 0° C., pyridine (40 mL, 5.0 eq) and acetic anhydride (47 mL, 5.0 eq) were added dropwise. The mixture was stirred for 8 h at room temperature. The reaction mixture was diluted with EtOAc and washed with H2O. The organic layer was dried over MgSO4 and concentrated in vacuo to give the desired product (20.0 g, 77%).

후처리

  1. washwashed with H2O
  2. dry with materialThe organic layer was dried over MgSO4
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-81ed5030ec0f49dc85e148b914b7501a
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877747B2

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