反应详情

The product of Example 1B (0.6 g, 0.842 mmole) was dissolved in 4 ml of methanol and 6 ml of THF. A solution of 180 mg of lithium hydroxide monohydrate in 1.5 ml of water was added and the mixture was refluxed for 5 hours. After cooling, 1 ml of concentrated hydrochloric acid was added and the mixture was stirred at room temperature for 2 hours. The resulting solution was concentrated under vacuum and 2 ml of water and 3 ml of ether was added to the residue. An oil which was insoluble in both layers formed. The oil was separated and crystallized from acetonitrile to provide 0.289 g of the desired product. M.p. 155°-158° C. 1H NMR (CD3OD) δ0.95 (t, 3H, J=7 Hz), 1.30 (m, 2H), 1.69 (m, 2H), 2.60 (s, 3H), 3.70 (m, 2H), 5.08 (m, 2H), 7.10 (d, 2H), 7.20 (s, 2H), 7.55 (d, 2H), 7.5-7.7 (m, 4H), 8.55 (s, 1H).

1. temperaturethe mixture was refluxed for 5 hours
2. temperatureAfter cooling
3. concentrationThe resulting solution was concentrated under vacuum and 2 ml of water and 3 ml of ether
4. additionwas added to the residue
5. customformed
6. customThe oil was separated
7. customcrystallized from acetonitrile