HRID1250590

反应详情

EQUATION

反应方程式

HRID 1250590 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 5 ml of a solution of 165 mg (0.67 mmol) of 2-allylamino-4-amino-6-nitroquinazoline in THF was added 17 mg (10.7 mmol) of sodium hydride. After the mixture was stirred under ice cooling for 0.5 hour, 76 mg (0.77 mmol) of t-butylisocyanate was added, followed by stirring for 1.5 hours at room temperature. After completion of the reaction, ice water was added to the reaction mixture, followed by extraction with chloroform (10 ml×3). After the organic layer was washed with brine and then dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by a silica gel chromatography to give 79 mg (yield: 34.2%) of the title compound.

WORKUP

后处理

  1. stirringby stirring for 1.5 hours at room temperature
  2. additionwas added to the reaction mixture
  3. extractionfollowed by extraction with chloroform (10 ml×3)
  4. washAfter the organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by a silica gel chromatography