反应详情

55 g (0.15 Mol) of the acid obtained in Example 2 are dissolved in 120 ml of toluene. Then 2 ml of pyridine and 40 ml of thionyl chloride are added thereto. This mixture is stirred for 3 hours at 80°. Then the solvents are distilled off under reduced pressure and the remaining oil (56 g) is dissolved in 200 ml of toluene. To this solution is added dropwise, at a temperature of 5°-15°, first 12.5 g of allyl alcohol, then 28 g of triethylamine. This reaction mixture is stirred overnight at room temperature and then added with 50 ml of water. The organic phase is separated, dried over sodium sulfate, filtered and then evaporated to dryness. The residue represents 57.8 g of a dark oil, which is dissolved in toluene and cleaned by chromatography over an alumina oxide column. After evaporation of the toluene and distillation, there remains 54 g of the allyl ester as a clear oil, b.p. 165° /0.01 torr.

1. distillationThen the solvents are distilled off under reduced pressure
2. dissolutionthe remaining oil (56 g) is dissolved in 200 ml of toluene
3. additionTo this solution is added dropwise, at a temperature of 5°-15°, first 12.5 g of allyl alcohol
4. stirringThis reaction mixture is stirred overnight at room temperature
5. additionadded with 50 ml of water
6. customThe organic phase is separated
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated to dryness
10. dissolutionis dissolved in toluene
11. customAfter evaporation of the toluene and distillation, there