HRID48274

反应详情

EQUATION

反应方程式

HRID 48274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Triethylamine (11.46 mL) was added to a suspension of 3-amino-6-methylquinolin-4-ol hydrochloride in dichloromethane (400 mL). Butyryl chloride (4.46 mL) was added. The reaction mixture was heated on a steam bath for 30 minutes. The solution was diluted with sodium bicarbonate and then filtered. The filtrate was washed with bicarbonate and then concentrated under vacuum. The residue was recrystallized from isopropanol to provide 3-butyramido-6-methylquinolin-4-ol hemihydrate as a solid, m.p. 274-277° C. Analysis: Calculated for C14H16N2O2.½ H2O: %C, 66.39; %H, 6.76; %N, 11.06; Found: %C, 66.56; %H, 6.46; %N, 11.03.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated on a steam bath for 30 minutes
  2. filtrationfiltered
  3. washThe filtrate was washed with bicarbonate
  4. concentrationconcentrated under vacuum
  5. customThe residue was recrystallized from isopropanol