反应详情

To a solution of about 14.53 g of lithium borohydride in about 630 ml of tetrahydrofuran at about 0° C. was added about 84.0 g of dimethyl[(2-methyl-1,3-dithiolan-2-yl)methyl]propanedioate dropwise. After the exotherm ended the mixture was stirred at room temperature for about 18 hours, then about 4.15 g of lithium borohydride were added and stirring was continued for about 20 hours. The solution was cooled in an ice bath, about 400 ml of about 6N hydrochloric acid were added dropwise, the mixture was saturated with sodium chloride and then extracted with ether. The ether layer was washed with brine, then saturated sodium bicarbonate, dried and the solvent removed. Methanol was added and removed three times. The solid was recrystallized from carbon tetrachloride, giving about 56.77 g of the desired title compound, mp 72°-73° C.

1. stirringstirring
2. waitwas continued for about 20 hours
3. temperatureThe solution was cooled in an ice bath
4. extractionextracted with ether
5. washThe ether layer was washed with brine
6. dry with materialsaturated sodium bicarbonate, dried
7. customthe solvent removed
8. additionMethanol was added
9. customremoved three times
10. customThe solid was recrystallized from carbon tetrachloride