反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureto reflux for 20 hours
- customAfter the solvent was evaporated in vacuo, water
- additionwas added to the residue
- extractionby extracting with chloroform
- washwashed with water
- dry with materiala saturated saline solution and dried over anhydrous sodium sulfate
- customthe solvent was evaporated in vacuo