反应详情

A mixture of 169 (56 mg, 0.22 mmol), 170 (42 mg, 0.25 mmol) and K2CO3 (138 mg) in DMF (4 mL) is stirred at room temperature overnight. Solvent is removed in vacuo. Water (10 mL) is added and the mixture is extracted with ethyl acetate (3×25 mL). The combined organic layers are dried and solvent removed. The crude is purified by PTLC (5% MeOH in methylene chloride) to give the title product (167) as a solid. 1H NMR 9.13 (s, 1H), 8.64–8.66 (m, 1H), 8.36 (s, 1H), 8.07–8.10 (m, 1H), 7.29–7.34 (m, 1H), 7.32 (s, 1H), 7.23 (s, 1H), 5.94 (s, 2H), 3.02–3.08 (m, 2H) 1.66–1.74 (m, 2H), 1.00 (t, 3H).

1. customSolvent is removed in vacuo
2. additionWater (10 mL) is added
3. extractionthe mixture is extracted with ethyl acetate (3×25 mL)
4. customThe combined organic layers are dried
5. customsolvent removed
6. customThe crude is purified by PTLC (5% MeOH in methylene chloride)