反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
A mixture of 3.02 g crude tert-butyl (1S,2S)-(6-fluoro-2-hydroxy-1-isopropyl-1, 2,3,4-tetrahydronaphthalen-2-yl)acetate and 8 mL 96% formic acid was stirred at 25° C. for four hours. The solution was diluted with 6 mL water; then heated to 75° C and filtered. The filtrate was slowly cooled to 25° C. with stirring. The resulting suspension was cooled to 0° C., stirred for one hour, and suction filtered. The precipitate was washed with 15 mL water, air dried at 25° C. for one hour, then oven dried at 50° C. for 22 hours to give 1.59 g (1S,2S)-(6-fluoro-2-hydroxy-l-isopropyl-1, 2,3,4-tetrahydronaphthalen-2-yl)acetic acid as a colorless solid, m.p. 102-103.5° C., [α]D27 = 78.80° (CHCl3).
WORKUP
后处理
- temperaturethen heated to 75° C
- filtrationfiltered
- temperatureThe filtrate was slowly cooled to 25° C.
- stirringwith stirring
- temperatureThe resulting suspension was cooled to 0° C.
- stirringstirred for one hour
- filtrationsuction filtered
- washThe precipitate was washed with 15 mL water, air
- customdried at 25° C. for one hour
- customoven dried at 50° C. for 22 hours