HRID430063
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 mixture of 2-chloro-4-methoxyquinoline (0.63 g, 3.25 mmol) and 2,2-dimethyl-1,3-propanediamine (2.00 g, 19.5 mmol) was stirred for 16 h at 75° C. in a sealed propanediamine (2.00 g, 19.5 mmol) was stirred for 16 h at 75° C. in a sealed NaHCO3 and ethyl acetate. The organic layer was dried (MgSO4) and concentrated onto silica, then chromatographed eluting with 5% then 10% methanol/CH2Cl2+0.5% 880 aqueous ammonia to give the title compound as a white solid (0.19 g, 23%). δH (CDCl3) 0.99 (6H, s, C(CH3)2), 2.57 (2H, s, 2′-H), 3.41 (2H, s, 4′-H), 3.96 (3H, s, OCH3), 5.98 (1H, s, 3-H), 7.12-7.93 (4H, m, ArH). MS (ES+) 260 (MH+).
WORKUP
后处理
- dry with materialThe organic layer was dried (MgSO4)
- concentrationconcentrated onto silica
- customchromatographed
- washeluting with 5%