反应详情

温度

0 °C

Ethyl ({[5,5-dimethyl-2-(4-methylphenyl)-1,3-dioxan-2-yl]methyl}thio)acetate (10.1 g, 29.8 mmol) was dissolved in THF (150 ml) and cooled to 0° C. LiOH (3.76 g, 89.5 mmol) in water (50 ml) was added and the mixture was stirred for two hours at room temperature. The mixture was concentrated under reduced pressure. Water was added and the mixture was extracted with diethyl ether. The aqueous layer was acidified using 2M HCl to pH 3 and extracted twice with CH2Cl2. The combined CH2Cl2 layers were dried (Na2SO4) and concentrated under reduced pressure to afford 8.7 g (94%) of the title compound as a white solid. 1H-NMR(CDCl3, 200 MHz): δ 0.6 (s, 3H), 1.2 (s, 3H), 2.4 (s, 3H), 3.0 (s, 2H), 3.4 (s, 2H), 3.4 (s, 4H), 7.2-7.4 (m. 4H).

1. concentrationThe mixture was concentrated under reduced pressure
2. additionWater was added
3. extractionthe mixture was extracted with diethyl ether
4. extractionextracted twice with CH2Cl2
5. dry with materialThe combined CH2Cl2 layers were dried (Na2SO4)
6. concentrationconcentrated under reduced pressure