HRID1881330

反应详情

EQUATION

反应方程式

HRID 1881330 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 473 mg (2.99 mmol) of 2-oxoindoline-5-carbonitrile in DMF (10 mL) were added 229 mg (5.73 mmol) of sodium hydride (60% on mineral oil) as a solid. After stirring the resulting suspension for 60 min at RT, a solution of 500 mg (2.49 mmol) of 6-chloro-N-methoxy-N-methylnicotinamide from example 1.1 in DMF (10 mL) was added slowly and the mixture was stirred for 80 min at 120° C. The reaction was cooled down to RT and a saturated solution of NH4CL (40 mL) was added and the resulting precipitate was collected by filtration. The precipitate was washed with water and hexane and afterwards dried in a vacuum oven. Yellow solid. Amount 265 mg. Yield 33%.

WORKUP

后处理

  1. stirringthe mixture was stirred for 80 min at 120° C
  2. temperatureThe reaction was cooled down to RT
  3. additiona saturated solution of NH4CL (40 mL) was added
  4. filtrationthe resulting precipitate was collected by filtration
  5. washThe precipitate was washed with water and hexane
  6. customafterwards dried in a vacuum oven