HRID574236
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
Benzyl 2-(benzyloxy)-3,3,3-trifluoro-2-methylpropanoate (Int. D3)(170 mg, 0.502 mmol) in MeOH (5 ml) was treated with 2M sodium hydroxide (0.502 ml, 1.005 mmol) 2M and stirred at RT for 2 h. The methanol was removed in vacuo and the residue was dissolved in water and washed with EtOAc. The aqueous phase acidified with 5M HCl and extracted with EtOAc. The combined organic extracts were washed with saturated brine, dried over magnesium sulfate and concentrated in vacuo afford the title product as a clear; 1H NMR (400 MHz, DMSO-d6) δ 14.08 (1H, br s), 7.35 (5H, m), 4.62 (2H, dd), 1.64 (3H, s).
WORKUP
后处理
- customThe methanol was removed in vacuo
- dissolutionthe residue was dissolved in water
- washwashed with EtOAc
- extractionextracted with EtOAc
- washThe combined organic extracts were washed with saturated brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo