HRID243079
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
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
- customThe volatiles were removed in vacuo
- dissolutionthe resulting residue dissolved in DCM
- washThe cartridge was washed with DCM
- concentrationThe relevant fractions were concentrated in vacuo