HRID55890
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
To a stirred solution of 53 (0.35 g, 2.2 mmol) in MeOH (6 mL) was added 10% Pd/C (50 mg) and hydrogenated using a balloon for 2 h at rt. The reaction mixture was filtered through a pad of Celite and concentrated to give the desired amine A4-18 (0.3 g, 69%) as a gummy liquid. Rf: 0.1 (10% MeOH/DCM); (m/z): 194 [MH]+; 1H NMR (400 MHz, DMSO-d6): δ 7.82 (1H, d, J=2.8 Hz), 6.95 (1H, d, J=8.4 Hz), 6.86 (1H, dd, J=8.4, 2.4 Hz), 5.12-5.10 (2H, m), 4.08 (1H, br s), 3.48 (2H, s), 3.16-3.14 (4H, m), 1.33 (3H, s).
WORKUP
后处理
- customfor 2 h
- customat rt
- filtrationThe reaction mixture was filtered through a pad of Celite
- concentrationconcentrated