HRID2281002

反应详情

EQUATION

反应方程式

HRID 2281002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-Bromoquinoline-8-carboxylic acid (30 g, 0.119 mol, crude) in DMF (400 ml) was added potassium carbonate (41.12 g, 0.297 mol) and MeI (22.3 ml, 0.357 mol) at RT. The reaction mixture was stirred at RT for 12 h and the reaction completion was confirmed by TLC. After completion of reaction the reaction mixture was filtered and evaporated. The reaction mixture was basified with 10% NaHCO3 and extracted with ethyl acetate. The organic layer was washed with water, brine and dried over sodium sulphate and concentrated to afford the title compound as brown liquid (4.6 g). LCMS: Mass found (M+, 268). 1H NMR (DMSO-d6 400 MHz): δ 9.04-9.02 (dd, J=3.92, 5.68, Hz, 1H), 8.58-8.56 (m, 1H), 8.05-8.03 (d, J=7.72 Hz, 1H), 7.87-7.86 (d, J=7.76 Hz, 1H), 7.78-7.75 (dd, J=8.6, 12.8 Hz, 1H), 3.91 (s, 3H).

WORKUP

后处理

  1. customAfter completion of reaction the reaction mixture
  2. filtrationwas filtered
  3. customevaporated
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with water, brine
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated