HRID1820119
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Zinc dust (10 g) was added in portions over 10 minutes to 2-cyclopentyl-N-(2,6-dimethyl-4-nitro-phenyl)-acetamide (1.45 g) in tetrahydrofuran (40 mL) and acetic acid (10 mL) cooled to 0° C. The reaction mixture was stirred 2 hours at 25° C., neutralized with solid sodium carbonate and filtered through silica (50 g), which was washed with ethyl acetate (200 mL). The organic phase was concentrated in vacuo to furnish 1.15 g (89% yield) of the title compound as a light orange solid. 1H NMR (500 MHz, DMSO-d6): 1.20 (m, 2H), 1.51 (m, 2H), 1.60 (m, 2H), 1.75 (m, 2H), 1.96 (s, 6H), 2.22 (m, 1H), 2.23 (d, 2H), 4.81 (b, 2H), 6.23 (s, 2H), 8.74 (s, 1H).
WORKUP
后处理
- filtrationfiltered through silica (50 g), which
- washwas washed with ethyl acetate (200 mL)
- concentrationThe organic phase was concentrated in vacuo