Chromanone → Benzopyran
반응식
[CH:1]1[CH:2]=[CH:3][C:4]2[O:11][CH2:10][CH2:9][C:7](=O)[C:5]=2[CH:6]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C(OCC)C>[O:11]1[C:4]2[C:5](=[CH:6][CH:1]=[CH:2][CH:3]=2)[CH:7]=[CH:9][CH2:10]1참가 물질
4
실험 절차
The chromanone was dissolved in 400 ml. of dry ethyl ether, and 2.5 gm of lithium aluminum hydride was added in portions. The reaction was refluxed for 2 hours and then allowed to come to room temperature. The excess lithium aluminum hydride was destroyed by dropwise addition of water and 150 ml. of 4N HCl was added slowly to the reaction mixture. Stirring was continued for 15 minutes. The reaction mixture was extracted with ether and washed successively with 100 ml. of water, 100 ml. 5% sodium carbonate solution and 100 ml. saturated NaCl solution. The ethereal extract was dried over anhydrous sodium sulfate. Removal of the ether in vacuo gave 15.6 g of crude chromene.
후처리
- temperatureThe reaction was refluxed for 2 hours
- customto come to room temperature
- customThe excess lithium aluminum hydride was destroyed by dropwise addition of water and 150 ml
- additionof 4N HCl was added slowly to the reaction mixture
- extractionThe reaction mixture was extracted with ether
- washwashed successively with 100 ml
- extractionThe ethereal extract
- dry with materialwas dried over anhydrous sodium sulfate
- customRemoval of the ether in vacuo
출처 및 근거
- ORD 기록
- ord-d0b784848fe449c8a22679f9a58c46d2
- 출처 데이터셋
- uspto-grants-1987_04
- 특허 번호
- US04656189
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