14 g of the acetyl compound of the formula (102) are suspended in 100 ml of deionized water at 20.degree. C. using a wetting agent. 29 g of 70% 3-chloroperbenzoic acid (MCPBA) are scattered in and the mixture is heated with stirring. A resin/water phase is formed from 52.degree. C.; the mixture is heated to about 80.degree. C. and kept at this temperature for 7 hours.
It is treated with 0.5 g of sodium hydrogen sulfite to destroy excess peroxide. Two clear phases are obtained by addition of 50 ml of xylene isomer mixture and 9 g of 10N NaOH. The water phase having a pH of about 12 is separated off; the solvent phase comprising the compound of the formula (103) is washed with water until neutral.
To hydrolyse the ester, the xylene phase is treated with 24 g of 10% NaOH and stirred under reflux (about 95.degree. C.) for 5 hours. The xylene phase is then separated off and the pale brown water phase is adjusted to a pH of about 3 using 4 g of 34% hydrochloric acid at 25.degree. C. In the course of this, the product precipitates in sandy, beige-coloured form and, after filtration, can be thoroughly washed with water on the suction filter. After drying, 5 g of the crude product of the formula (104) having a melting point of 73 to 74.degree. C. are obtained.
After recrystallization from petroleum ether 80/110, the pure substance is obtained in colourless crystals having a melting point of 74 to 74.5.degree. C，
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是Baeyer-Villing反应么，那个很容易呀，是制备酚或羟基的一条很好的间接路线
给你个例子:US6706930
14 g of the acetyl compound of the formula (102) are suspended in 100 ml of deionized water at 20.degree. C. using a wetting agent. 29 g of 70% 3-chloroperbenzoic acid (MCPBA) are scattered in and the mixture is heated with stirring. A resin/water phase is formed from 52.degree. C.; the mixture is heated to about 80.degree. C. and kept at this temperature for 7 hours.
It is treated with 0.5 g of sodium hydrogen sulfite to destroy excess peroxide. Two clear phases are obtained by addition of 50 ml of xylene isomer mixture and 9 g of 10N NaOH. The water phase having a pH of about 12 is separated off; the solvent phase comprising the compound of the formula (103) is washed with water until neutral.
To hydrolyse the ester, the xylene phase is treated with 24 g of 10% NaOH and stirred under reflux (about 95.degree. C.) for 5 hours. The xylene phase is then separated off and the pale brown water phase is adjusted to a pH of about 3 using 4 g of 34% hydrochloric acid at 25.degree. C. In the course of this, the product precipitates in sandy, beige-coloured form and, after filtration, can be thoroughly washed with water on the suction filter. After drying, 5 g of the crude product of the formula (104) having a melting point of 73 to 74.degree. C. are obtained.
After recrystallization from petroleum ether 80/110, the pure substance is obtained in colourless crystals having a melting point of 74 to 74.5.degree. C，