反应详情

To a solution of 5-methyl-2-trifluoromethyl-furan-3-carboxylic acid ethyl ester (0.83 g, 3.7 mmol) in Et2O at 0° C., was added DIBAL-H (1.0 M in THF, 1.5 mL). After 10 min, the ice bath was removed and additional DIBAL-H was added (1.0 M in THF, 14.5 mL). After 2 h, the reaction was quenched with a saturated solution of sodium potassium tartrate (aq.) and allowed to stir overnight. After 18 h, EtOAc was added and the organic layer separated and dried provide the title compound (0.39 g, 58%). 1H NMR (CDCl3): 6.19 (s, 1H), 4.62 (s, 2H), 2.36-2.28 (m, 3H).

1. customthe ice bath was removed
2. additionadditional DIBAL-H was added (1.0 M in THF, 14.5 mL)
3. waitAfter 2 h
4. customthe reaction was quenched with a saturated solution of sodium potassium tartrate (aq.)
5. waitAfter 18 h
6. additionEtOAc was added
7. customthe organic layer separated
8. customdried