反应详情

To a solution of compound from Step 2 (5.57 g, 15.96 mmol) in THF (40 mL) them was added n-Bu4NF 1M in THF (18 mL); the mixture was stirred at r.t. for 30 min., then H2O (10 mL) was added. The mixture was concentrated to a small volume, the residue extracted with EtOAc, the extract washed twice with brine, dried and evaporated to a residue which was chromatographed on silica gel, eluting with a 1:1 mixture of EtOAc and hexane, to afford the title product as a white solid (2.59 g) m.p. 145°-146° C.

1. concentrationThe mixture was concentrated to a small volume
2. extractionthe residue extracted with EtOAc
3. washthe extract washed twice with brine
4. customdried
5. customevaporated to a residue which
6. customwas chromatographed on silica gel
7. washeluting with a 1:1 mixture of EtOAc and hexane