반응식
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]=1[C:13]([O:15]C)=[O:14].[OH-].[K+].CO.Cl>O.C(O)C>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]=1[C:13]([OH:15])=[O:14]참가 물질
7
반응 조건
- 온도
- 0 °C
실험 절차
A solution of 21.6 g of the compound of Step A above in 48 ml of Claisen's alkali solution (solution of 21 g of KOH in 15 ml of water, made up to 60 ml with methanol) is heated at reflux for 4 hours. The reaction mixture is then diluted with 50 ml of water and poured into 75 ml of 15.5% hydrochloric acid solution cooled to 0° C. with stirring. The white precipitate formed is then filtered off over a Buchner funnel and then washed with water and dried under a phosphoric vacuum. The dry residue obtained is dissolved in a solution of ethanol and water (80:20, v/v) at boiling. After cooling to 0° C., 13.7 g of the expected product are obtained.
후처리
- temperatureis heated
- temperatureat reflux for 4 hours
- customThe white precipitate formed
- filtrationis then filtered off over a Buchner funnel
- washwashed with water
- customdried under a phosphoric vacuum
- customThe dry residue obtained
- temperatureAfter cooling to 0° C.
출처 및 근거
- ORD 기록
- ord-69dc9baf0c6746dda3fdcdb16b21c03a
- 출처 데이터셋
- uspto-grants-2007_10
- 특허 번호
- US07276512B2
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