HRID1432855

反应详情

EQUATION

反应方程式

HRID 1432855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-chloro-2-methyl-1,2,3,4-tetrahydronaphthalene-2-ol (11.3 g, 57.5 mmol) and Ph3COH (16.5 g, 63 mmol) in 80 mL of TFA is stirred for 2.5 days. After this time, the solution is concentrated to dryness. The residue is dissolved in CH2Cl2. The organic layer is washed with H2O, saturated NaHCO3, and saturated NaCl. The organic layer is dried over MgSO4, filtered and concentrated. The crude product is purified by column chromatography eluting with hexanes. The title compound is obtained as a white solid (4.05 g, 22.9 mmol). 1H NMR (CDCl3, 300 MHz) δ7.78 (s, 1H), 7.69 (m, 2H), 7.58 (s, 1H), 7.50 (m, 2H), 2.49 (s, 3H).

WORKUP

后处理

  1. concentrationAfter this time, the solution is concentrated to dryness
  2. dissolutionThe residue is dissolved in CH2Cl2
  3. washThe organic layer is washed with H2O, saturated NaHCO3, and saturated NaCl
  4. dry with materialThe organic layer is dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude product is purified by column chromatography
  8. washeluting with hexanes