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
After dissolving 4-{[({[2-(carbamoylmethyl)phenyl]amino}thioxomethyl)amino]methyl}piperidine carboxylic acid tert-butyl ester (410 mg, 1.01 mmol) in tetrahydrofuran (15 mL), N,N′-dicyclohexylcarbodiimide (208 mg, 1.01 mmol) was added and the mixture was stirred at room temperature for 6 hours. The filtrate obtained by filtering the insoluble portion was concentrated under reduced pressure, and the concentrate was suspended in a solution of n-hexane:ethyl acetate=1:2 (3 mL). The insoluble portion was refiltered, and the residue obtained by concentrating the filtrate under reduced pressure was purified by silica gel column chromatography (n-hexane/ethyl acetate=2/3→1/2) to obtain the title compound. Yield: 193 mg (51%).
WORKUP
后处理
- additionwas added
- customThe filtrate obtained
- filtrationby filtering the insoluble portion
- concentrationwas concentrated under reduced pressure
- customthe residue obtained
- concentrationby concentrating the filtrate under reduced pressure
- customwas purified by silica gel column chromatography (n-hexane/ethyl acetate=2/3→1/2)