反应详情

In a method similar to Example 5, the product of Example 1, Step 2 (0.218 g, 0.500 mmol) was converted to the title compound with pyrrolidine (0.053 g, 0.780 mmol) in 1 hour to give 0.34 g of product which was purified by flash column (3:2 hexane/ethyl acetate) to afford 0.17 (74%) of white solid after recrystallization: mp 243°-245° C.; 1H NMR (DMSO-D6): δ 7.74 (d, 1H), 7.29 (d, 1H), 7.18 (dd, 1H), 6.89 (d, 1H), 5.81 (d, 1H), 4.94 (t, 1H), 4.00 (m, 1H), 3.87 (m, 2H), 3.57 (m, 2H), 2.10-1.90 (m, 4H), 1.41 (s, 3H), 1.17 (s, 3H); IR (KBr): 3350, 1595 cm-1 ; MS (m/z) 463 (MH +, 100%); [α]D25 =-75.5 (THF).