反应详情

To a mixture of the product from step c) (0.34 g) and benzenesulfonyl chloride (0.11 ml) in THF (3 ml) was added triethylamine (0.42 ml) dropwise. After 5 min, further THF (3 ml) was added and the reaction stirred for 16 h. It was poured into 2M HCl and extracted with ethyl acetate. The organic layer was separated and washed with sat aqueous sodium bicarbonate solution, brine, dried (Na2SO4) and the solvent removed in vacuo. The residue was stirred in THF (2 ml) and 4M NaOH (4 ml) for 16 h. After acidification to pH 3, the aqueous layer was extracted with ethyl acetate. The organic layer was separated and the solvent removed in vacuo. Purification by RPHPLC (symmetry column) gave the title product as a white foam (0.12 g).

1. extractionextracted with ethyl acetate
2. customThe organic layer was separated
3. washwashed with sat aqueous sodium bicarbonate solution, brine
4. dry with materialdried (Na2SO4)
5. customthe solvent removed in vacuo
6. stirringThe residue was stirred in THF (2 ml)
7. wait4M NaOH (4 ml) for 16 h
8. extractionAfter acidification to pH 3, the aqueous layer was extracted with ethyl acetate
9. customThe organic layer was separated
10. customthe solvent removed in vacuo
11. customPurification by RPHPLC (symmetry column)