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[C:1]([C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:15][CH3:16])[C:10]=2[Br:14])[CH:5]=1)(=[O:3])[CH3:2].C[O-].[Na+].Cl.[C:21](OCC)(=[O:23])[CH3:22]>>[Br:14][C:10]1[C:9]([O:15][CH3:16])=[CH:8][CH:7]=[C:6]2[C:11]=1[CH:12]=[CH:13][C:4]([C:1]([OH:3])=[CH:2][C:21](=[O:23])[CH3:22])=[CH:5]2참가 물질
실험 절차
139.4 Grams (0.499 moles) of 2-acetyl-5-bromo-6-methoxynaphthalene and 1450 ml of ethyl acetate are placed in a flask equipped with refrigerator and stirrer and, under stirring and at the temperature of 45° C., 30 g (0.556 moles) of sodium methoxide are added. The temperature of the reaction mixture goes up to 55° C. and is kept at 65° C. for one hour, then other 10 g (0.185 moles) of sodium methoxide are added and, after half an hour, still other 10 g (0.185 moles) of sodium methoxide, always under stirring and keeping the temperature at 65° C. for another hour and half. The reaction mixture is then cooled to room temperature and brought to pH 4 by adding a concentrated aqueous solution of hydrochloric acid. The reaction mixture is then heated to reflux for 15 minutes, cooled to 5° C. in one hour and kept at this temperature for 2 hours. The precipitated solid is filtered, abundantly washed with water on the filter, then washed with ethyl acetate and dried in oven under vacuum obtaining 145.7 g of product with a yield equal to 90.8%.
후처리
- customequipped with refrigerator and stirrer
- additionare added
- customgoes up to 55° C.
- customat 65° C.
- temperatureThe reaction mixture is then heated
- temperatureto reflux for 15 minutes
- temperaturecooled to 5° C. in one hour
- waitkept at this temperature for 2 hours
- filtrationThe precipitated solid is filtered
- washabundantly washed with water on the filter
- washwashed with ethyl acetate
- customdried in oven under vacuum
출처 및 근거
- ORD 기록
- ord-530a7141e8bf4163aca3b64b90bcb690
- 출처 데이터셋
- uspto-grants-1998_05
- 특허 번호
- US05750793
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