HRID1594507
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
The title compound of Example 6, Step A (150 mmol, 33 g) and Pearlman's catalyst (ca. 400 mg) were agitated in MeOH (200 mL) under H2 (40 psi, Parr shaker) for 4 h. The reaction mixture was filtered through celite and the filtrate was concentrated in vacuo. Flash chromatography on silica eluting with 20-25% EtOAc in hexanes afforded the product as a light orange solid. 1H NMR (500 MHz, CDCl3), δ (ppm): 7.17 (1H, d, J=8.3 Hz), 6.97 (1H, d, J=1.9 Hz), 6.68 (1H, d, J=8.2 Hz), 3.78 (1H, bs), 3.38 (2H, bs), 2.94 (3H, s). LC-MS (ESI, Method C): 2.71, m/z 191.1 (M+1).
WORKUP
后处理
- filtrationThe reaction mixture was filtered through celite
- concentrationthe filtrate was concentrated in vacuo