反应详情

Compound 36a (5.1 g, 11.5 mmol) was dissolved in 40 ml of dichloromethane and 40 ml of trifluoroacetic acid was added. The mixture was stirred for 3 hr, at which time the solution was concentrated to dryness, dissolved in sat. NaHCO3, and extracted with EtOAc. The organic layer was dried (Na2SO4), filtered, and concentrated to yield 3.8 g (96%) of 37a, which was used as is in the next reaction. 1H NMR (400 MHz, CDCl3) 0.93-0.96 (t, 3H, J=7.6 Hz), 1.62 (m, 3H), 1.85-1.97 (m, 3H), 2.56 (m, 1H), 2.81-2.88 (m, 5H), 2.98-3.34 (m, 9H), 3.81 (s, 3H), 6.60-6.61 (dd, 1H, J=1.6 Hz), 6.65-6.78 (m, 1H), 6.95-6.98 (d, 1H, J=8.8 Hz).

1. concentrationwas concentrated to dryness
2. dissolutiondissolved in sat. NaHCO3
3. extractionextracted with EtOAc
4. dry with materialThe organic layer was dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated