HRID710473
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
A solution of the product of Step A (0.25 g; 1.55 mmol), 10% Pd/C (0.15 g) and triethylamine (0.5 ml) in EtOH (15 ml) was stirred overnight at room temperature under H2 (Parr apparatus; 100 psi). The catalyst was removed by filtration, washed with fresh EtOH (2×10 ml), and combined filtrates were evaporated to dryness to give the title compound (0.25 g; 100%), as greyish solid, which was used in the next Step without further purification. 1H-NMR (CDCl3) 0.94 (tr, 3H, J=6 Hz); 1.69-1.81 (m, 2H); 2.83 (tr, 2H, J=6 Hz); 7.2 (d, 1H, J=9 Hz); 8.19 (s, 1H); 8.28 (d, 1H, J=9 Hz); 10.65 (broad s, 1H).
WORKUP
后处理
- customThe catalyst was removed by filtration
- washwashed with fresh EtOH (2×10 ml)
- customwere evaporated to dryness