反应详情

Di-tert-butyl[2-(ethoxycarbonyl)-1-benzothien-6-yl](fluoro)malonate (9.3 g) was stirred in DCM (40 mL)/TFA (20 mL) at room temperature overnight. The solvent was removed in vacuo and the residue partitioned between saturated NaHCO3-EtOAc. The aqueous phase was acidified with 2N HCl and extracted with EtOAc. The combined organic extracts were dried over MgSO4 and concentrated in vacuo. The residue was suspended in H2O (50 mL) and heated to reflux for 2 hours. Room temperature was attained and the products extracted into EtOAc. The combined organic extracts were dried over MgSO4 and concentrated in vacuo to give the product as a pale yellow solid. 1H NMR (DMSO-d6) δ 13.60 (br s, 1H), 8.22 (s, 1H), 8.18 (s, 1H), 8.08 (d, J=8.4 Hz, 1H), 7.51 (d, J=8.4 Hz, 1H), 6.14 (d, J=47.4 Hz, 1H), 4.35 (q, J=7.2 Hz, 2H), 1.33 (t, J=7.2 Hz, 3H).

1. customThe solvent was removed in vacuo
2. customthe residue partitioned between saturated NaHCO3-EtOAc
3. extractionextracted with EtOAc
4. dry with materialThe combined organic extracts were dried over MgSO4
5. concentrationconcentrated in vacuo
6. temperatureheated
7. temperatureto reflux for 2 hours
8. customRoom temperature
9. extractionthe products extracted into EtOAc
10. dry with materialThe combined organic extracts were dried over MgSO4
11. concentrationconcentrated in vacuo