HRID1194290
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
First, 3 g of 2-methylthiocycloheptimidazole as synthesized according to Synthetic example 1 (c) with reference to the method disclosed in Bulletin of the Chemical Society of Japan, volume 33, No. 1, pages 56 to 58 (1960) was added to 50 ml of methanol, and 1 g of sodium methoxide was further added thereto. After reflux with heating for 10 hours, the solvent was distilled away, and 50 ml of benzene was added to the residue. The insoluble matters were filtered out, and the filtrate was concentrated. The resulting crystals were purified by silica gel column chromatography using ethyl acetate as a developing solvent.
WORKUP
后处理
- additionwas further added
- temperatureAfter reflux
- temperaturewith heating for 10 hours
- distillationthe solvent was distilled away
- addition50 ml of benzene was added to the residue
- filtrationThe insoluble matters were filtered out
- concentrationthe filtrate was concentrated
- customThe resulting crystals were purified by silica gel column chromatography