8-methoxy-2H-chromene → HCID 13758736, 화합물
반응식
[CH3:1][O:2][C:3]1[C:12]2[O:11][CH2:10][CH:9]=[CH:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[H][H]>C(O)(=O)C.[Pd]>[CH3:1][O:2][C:3]1[C:12]2[O:11][CH2:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1참가 물질
5
실험 절차
The compound obtained in Step B (1 g:6.84 mmol) dissolved in glacial acetic acid (10 ml) is poured into the reactor of a Paar apparatus. 10% palladium on carbon (10% by weight; 100 mg), acting as catalyst, is added. The whole is then subjected to a hydrogen pressure of 45 psi for 12 hours at room temperature. After filtration, the solvent is removed under reduced pressure and then extraction is carried out with dichloromethane. The recovered organic phase, dried over magnesium sulphate, is purified after concentration over a silica column eluted with pure dichloromethane. The title product is obtained pure in the form of a yellow oil.
후처리
- additionis poured into the reactor of a Paar apparatus
- additionis added
- filtrationAfter filtration
- customthe solvent is removed under reduced pressure
- extractionextraction
- dry with materialThe recovered organic phase, dried over magnesium sulphate
- customis purified
- concentrationafter concentration over a silica column
- washeluted with pure dichloromethane
출처 및 근거
- ORD 기록
- ord-6eb18eefd2fe4e75b69526204d65328d
- 출처 데이터셋
- uspto-grants-1999_07
- 특허 번호
- US05919814
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