HRID1027902
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 Example 118A (170 mg, 0.7 mmol) in methanol (15 mL) was treated with Raney nickel (slurry in H2O, 1 spatula) and refluxed for 16 hours. The mixture was filtered through diatomaceous earth and washed with methanol. The filtrate was concentrated under vacuum to provide the title compound. 1H NMR (CD3OD) δ 2.24 (t, 2H), 2.40 (t, 2H), 2.59 (t, 2H), 7.27-7.34 (m, 1H), 7.36-7.42 (m, 2H), 7.60-7.66 (m, 1H), 8.14-8.18 (m, 1H). MS (M+H)+ m/z 213
WORKUP
后处理
- temperaturerefluxed for 16 hours
- filtrationThe mixture was filtered through diatomaceous earth
- washwashed with methanol
- concentrationThe filtrate was concentrated under vacuum