HRID243079

反应详情

EQUATION

反应方程式

HRID 243079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (cis-3-benzyloxycyclobutyl)carbamic acid tert-butyl ester (2.40 g, 8.67 mmol) in DCM (20 mL) was added TFA (4 mL) and the mixture stirred at RT for 3 h. The volatiles were removed in vacuo and the resulting residue dissolved in DCM and loaded onto SCX-2 (20 g). The cartridge was washed with DCM then MeOH then 2M NH3 in MeOH solution. The relevant fractions were concentrated in vacuo to afford the title compound as yellow oil (1.48 g, 95%). 1H NMR (CDCl3, 400 MHz): δ 7.36-7.30 (5H, m), 4.40 (2H, s), 3.73-3.61 (1H, m), 3.06-2.93 (1H, m), 2.72-2.58 (2H, m), 1.74-1.61 (2H, m), 1.47 (2H, s, br).

WORKUP

后处理

  1. customThe volatiles were removed in vacuo
  2. dissolutionthe resulting residue dissolved in DCM
  3. washThe cartridge was washed with DCM
  4. concentrationThe relevant fractions were concentrated in vacuo