反应详情

Water is azeotropically removed from a solution of p-toluenesulfonic acid monohydrate in toluene (150 g) until the distillate is clear. A solution of 1-[1-(p-chlorophenyl)-2,2-dimethoxyethyl]cyclopropane (24.7 g, 0.1 mol) in toluene is then added to the dried solution at 100° C. The resultant reaction mixture is refluxed for one hour, distilled to remove about 80 g of toluene/methanol, cooled to room temperature, treated with sodium carbonate (1 g), and poured into a saturated bicarbonate solution (100 mL). The organic phase is separated, washed with water, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product (20 g, 96% yield).

1. customWater is azeotropically removed from a solution of p-toluenesulfonic acid monohydrate in toluene (150 g) until the distillate
2. customThe resultant reaction mixture
3. temperatureis refluxed for one hour
4. distillationdistilled
5. customto remove about 80 g of toluene/methanol
6. additiontreated with sodium carbonate (1 g)
7. additionpoured into a saturated bicarbonate solution (100 mL)
8. customThe organic phase is separated
9. washwashed with water
10. dry with materialdried over anhydrous magnesium sulfate
11. concentrationconcentrated in vacuo