反应详情

S1 was synthesized as reported procedure. Zhang, Z.; Achilefu, S. Org. Lett., 2004, 6, 2067-2070. A solution of POCl3 (37 mL, 397 mmol) in CH2Cl2 (35 mL) was slowly added to an ice-cooled solution of DMF (40 mL, 516 mmol) in CH2Cl2 (40 mL). After the addition was finished, cyclohexanone (10 g, 100 mmol) was added dropwisely. The resulted reaction mixture was refluxed for 2 h. The mixture was then cooled in ice. Water (200 mL) was added slowly while the mixture was stirred. The mixture was stirred for 1 h. The organic layer was collected and the water layer was extracted with additional CH2Cl2 (40 mL×3). The combined organic layers were dried over Na2SO4 and then evaporated. The residue was taken up in a mixture of AcOEt-diethylether (3:1), and the mixture was washed with water (30 mL×5) to remove DMF. The combined organic layers were dried over Na2SO4 and then evaporated. The residue was treated with pentane (200 mL) to give 4.2 g (23%) of S1 as yellow crystalline solid. LRMS (ESI): calculated for [(M+H)+] 173.1. found 173.1.

1. customS1 was synthesized
2. additionAfter the addition
3. customThe resulted reaction mixture
4. temperaturewas refluxed for 2 h
5. temperatureThe mixture was then cooled in ice
6. stirringThe mixture was stirred for 1 h
7. customThe organic layer was collected
8. extractionthe water layer was extracted with additional CH2Cl2 (40 mL×3)
9. dry with materialThe combined organic layers were dried over Na2SO4
10. customevaporated
11. additionThe residue was taken up in a mixture of AcOEt-diethylether (3:1)
12. washthe mixture was washed with water (30 mL×5)
13. customto remove DMF
14. dry with materialThe combined organic layers were dried over Na2SO4
15. customevaporated
16. additionThe residue was treated with pentane (200 mL)
17. customto give 4.2 g (23%) of S1 as yellow crystalline solid