HRID1181844

反应详情

EQUATION

反应方程式

HRID 1181844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

5-Chloro-1H-indole-3-carbaldehyde(3-isobutyl-1-methyl-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-yl)hydrazone (100 mg) was added to a solution of isoxazolaldehyde (86 mg) in dimethylformamide at RT. Piperidine (100 uL) was then added and brought to 80 C for 8 h. After cooling to RT, ethyl acetate (25 mL) was added to brown solution and water (25 mL) was added and extracted. The aqueous layer was back extract with ethyl acetate and then combined. The organic layer was dried over sodium sulfate, filtered and removal of solvent to give an amorphous solid. The isoxazole was submitted the Gilson Preparatory chromatography to give a 100 mg of white solids. ES M+H+467.

WORKUP

后处理

  1. additionwas added
  2. extractionextracted
  3. extractionThe aqueous layer was back extract with ethyl acetate
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. customremoval of solvent
  7. customto give an amorphous solid