HRID60246
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 (1-ethylpiperidin-4-yl)-methylcarbamic acid tert-butyl ester (1.65 g, 6.8 mmol) in dichloromethane (15 mL) was added TFA (5 mL). After 1 hour at ambient temperature the reaction mixture was concentrated in-vacuo and the residue loaded onto a 70 g SCX-2 cartridge which was washed with methanol, then 2N ammonia in methanol. Concentration of the combined basic fractions in-vacuo afforded the title compound as an orange oil (900 mg, 94%). 1H NMR (300 MHz, CD3OD): 2.95 (d, J=11.6 Hz, 2H), 2.48-2.36 (m, 3H), 2.35 (s, 3H), 1.96-1.95 (m, 4H), 1.40-1.38 (m, 2H), 1.09 (t, J=7.2 Hz, 3H).
WORKUP
后处理
- concentrationAfter 1 hour at ambient temperature the reaction mixture was concentrated in-vacuo
- washwas washed with methanol