HRID1900752
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
A mixture of 2-bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one (4.802 g) and thiazoline (5.815 g) was stirred at 150° C. in the stream of argon gas for 4 hours. The solvent was distilled off under reduced pressure. Chloroform was added to the residue, and extracted with 1N-HCl. After the extract was washed with chloroform, 1N-NaOH was added to bring the pH basic. Extraction was performed with chloroform, followed by washing with water. After dried, the residue was crystallized from methanol to obtain 1.885 g of a free base of the title compound as pale yellow powder (mp.: 196°-199° C.).
WORKUP
后处理
- distillationThe solvent was distilled off under reduced pressure
- additionChloroform was added to the residue
- extractionextracted with 1N-HCl
- washAfter the extract was washed with chloroform, 1N-NaOH
- additionwas added
- extractionExtraction
- washby washing with water
- customAfter dried
- customthe residue was crystallized from methanol