HRID2353603
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
The above [4-(2-hydroxy-ethoxy)-2-methoxy-benzyl]-carbamic acid tert-butyl ester (10.3 mg, 0.35 mmol) is treated with 37% aq. HCl (0.1 mL) and acetic acid (1 mL) for 1.5 h at rt. The solvents are removed by lyophilisation. The residue is dissolved in 2 N aq. NaOH (1 mL) and ethanol (0.25 mL) and heated to 80° C. for 1 h. The mixture is cooled to rt and extracted twice with EA. The organic extracts are combined, dried over Na2SO4, filtered and evaporated to give 2-(4-aminomethyl-3-methoxy-phenoxy)-ethanol (6.4 mg) as a beige oil. LC-MS: tR=0.58 min, [M+1]+=198.11.
WORKUP
后处理
- customThe solvents are removed by lyophilisation
- dissolutionThe residue is dissolved in 2 N aq. NaOH (1 mL)
- temperatureThe mixture is cooled to rt
- extractionextracted twice with EA
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated