反应详情

温度

-30 °C

10.0 g (0.039 mole) of the crude acid chloride from (c), above, is dissolved in 200 ml of dry tetrahydrofuran and the solution placed in a 500 ml round bottom flask fitted with a septum inlet and magnetic stirrer, and held under a nitrogen atmosphere. The solution is cooled to -30° C. in a dry ice/isopropanol bath and 19.5 ml (0.039 mole) of a commercial 2 M methyl magnesium bromide solution in dry toluene is added, dropwise, over 30 minutes. After the addition is complete, the mixture is allowed to warm to room temperature and then stirred for 1 hour. The reaction is quenched by the addition of 20 ml of saturated ammonium chloride solution and the organic layer is separated. The aqueous layer is extracted twice with 20 ml portions of ether and the combined organic extracts are then dried over anhydrous magnesium sulphate and evaporated to yield the heading compound, m.p. 130° to 133° C., after recrystallisation from petroleum ether.

1. customthe solution placed in a 500 ml round bottom flask
2. customfitted with a septum inlet and magnetic stirrer
3. additionAfter the addition
4. temperatureto warm to room temperature
5. customThe reaction is quenched by the addition of 20 ml of saturated ammonium chloride solution
6. customthe organic layer is separated
7. extractionThe aqueous layer is extracted twice with 20 ml portions of ether
8. dry with materialthe combined organic extracts are then dried over anhydrous magnesium sulphate
9. customevaporated
10. customto yield the heading compound, m.p. 130° to 133° C.
11. customafter recrystallisation from petroleum ether