HRID2060860

反应详情

EQUATION

反应方程式

HRID 2060860 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 6-(5-methylnaphthalen-1-yloxy)nicotinonitrile (Preparation 22) (530 mg, 2.04 mmol) in carbon tetrachloride (30 mL) under argon was added N-bromosuccinimide (435 mg, 2.44 mmol) followed by benzoyl peroxide (25 mg, 0.1 mmol). The mixture was heated to 70° C. for 16 h. The reaction mixture was cooled, filtered through celite, and washed with DCM (70 mL). The organic phase was washed with NaHCO3 (30 mL), brine (30 mL) and dried (MgSO4). Solvent was removed in vacuo to give the title compound: RT=3.93 min; m/z (ES+)=341.0 [M+H]+.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. filtrationfiltered through celite
  3. washwashed with DCM (70 mL)
  4. washThe organic phase was washed with NaHCO3 (30 mL), brine (30 mL)
  5. dry with materialdried (MgSO4)
  6. customSolvent was removed in vacuo