HRID2353603

反应详情

EQUATION

反应方程式

HRID 2353603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvents are removed by lyophilisation
  2. dissolutionThe residue is dissolved in 2 N aq. NaOH (1 mL)
  3. temperatureThe mixture is cooled to rt
  4. extractionextracted twice with EA
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated