HRID1357877

反应详情

EQUATION

反应方程式

HRID 1357877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of acetic acid (10 mL) in H2O (60 mL), was added 7-[(tertbutyldimethylsilyl)oxy]-1-hydroxy-6-methoxy-1-(3′,4′,5′-trimethoxyphenyl)-tetralin (137 mg, 0.29 mmol). The solution was heated to reflux for 8 hour, and then cooled down to rt. NaHCO3 (20 mL, saturated solution) was added, and the mixture was partitioned between CH2Cl2 and water. The organic layer was dried over anhydrous sodium sulfate, and after filtration, the organic layer was concentrated in vacuo to provide a yellow oil. 7-Hydroxy-6-methoxy-1-(3′,4′,5′-trimethoxyphenyl)-3,4-dihydronaphthalene (84.3 mg, 0.25 mmol, 86%) was obtained following purification by column chromatography. 1H-NMR (CDCl3, 300 MHz) 2.37 (m, 2H), 2.78 (t, J=7.7 Hz, 2H), 3.84 (s, 6H), 3.88 (s, 3H), 3.91 (s, 3H), 5.41 (s, 1H), 5.98 (t, J=4.6 Hz, 1H), 6.54 (s, 2H), 6.68 (s, 1H), 6.81 (s, 1H).

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureto reflux for 8 hour
  3. customthe mixture was partitioned between CH2Cl2 and water
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationafter filtration
  6. concentrationthe organic layer was concentrated in vacuo
  7. customto provide a yellow oil