HRID548195

反应详情

EQUATION

反应方程式

HRID 548195 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(3,5-Bis(trifluoromethyl)benzyloxymethyl)-2-phenyl-[1,3]dioxolane (50.72 g, 140 mmol) was dissolved in THF (300 mL), 60 mol/L hydrochloric acid (50 mL) was added thereto and the mixture was heated to reflux for 20 hours. After the solvent was evaporated in vacuo, water was added to the residue followed by extracting with chloroform. The organic layers were combined, washed with water and a saturated saline solution and dried over anhydrous sodium sulfate and the solvent was evaporated in vacuo to give 2-(3,5-bis(trifluoromethyl)-benzyloxy)-1-phenylethanone (48.90 g, 96%) as an oily product. 1H-NMR (DMSO-d6) δ: 4.82 (s, 2H), 5.07 (s, 2H), 7.53-7.57 (m, 2H), 7.66-7.69 (m, 1H), 7.94-7.96 (m, 2H), 8.03 (s, 1H), 8.11 (s, 2H).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 20 hours
  3. customAfter the solvent was evaporated in vacuo, water
  4. additionwas added to the residue
  5. extractionby extracting with chloroform
  6. washwashed with water
  7. dry with materiala saturated saline solution and dried over anhydrous sodium sulfate
  8. customthe solvent was evaporated in vacuo