HRID2427757
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 7-chloro-5-ethynyl-2-(4-trifluoromethoxy-benzyl)-2,3-dihydro-isoindol-1-one (0.080 g, 0.22 mmol) in ethanol (25 mL) was treated with 10% palladium on carbon (20 mg) and shook vigorously under 45 p.s.i. hydrogen for 2-3 h. The resulting mixture was filtered through Celite and the filtrate concentrated under reduced pressure. Silica gel column chromatography using combinations of hexane-ethyl acetate (typically 3:1 hexane-ethyl acetate) afforded 7-chloro-5-ethyl-2-(4-trifluoromethoxy-benzyl)-2,3-dihydro-isoindol-1-one (0.051 g, 63%). 1H NMR (300 MHz, CDCl3): δ (ppm) 1.28 (t, 3H), 2.74 (q, 2H), 4.23 (s, 2H), 4.81 (s, 2H), 7.12-7.39 (m, 6H). GC-MS: m/z 369 (M)+, 300 (M−69)+.
WORKUP
后处理
- filtrationThe resulting mixture was filtered through Celite
- concentrationthe filtrate concentrated under reduced pressure