反应详情

Lithium aluminum hydride (5.84 mL, 5.84 mmol, 1.0 M solution in Et2O) was added to a solution of 10 (595 mg, 2.59 mmol) in THF (12 mL) under argon. The reaction was then heated at reflux for 15 min, quenched by careful addition of H2O followed by 1 M NaOH, then extracted with CH2Cl2 (3×). The combined organic layers were dried over Na2SO4 and evaporated to afford 11 (490 mg, 94%) as a brown oil which was used without further purification; 1H NMR (CDCl3): δ 6.95 (1H, d), 6.71 (1H, d), 6.34 (1H, s), 4.77 (2H, s), 3.87 (3H, s), 3.74 (3H, s).

1. temperatureThe reaction was then heated
2. temperatureat reflux for 15 min
3. customquenched by careful addition of H2O
4. extractionextracted with CH2Cl2 (3×)
5. dry with materialThe combined organic layers were dried over Na2SO4
6. customevaporated