HRID1168103
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
A solution of the title compound of Step A (20 mg, 0.055 mmol) and sulfur monochloride (26.7 μl, 0.33 mmol) in ethyl acetate/acetic acid (2.4 ml/0.6 ml) was heated to reflux for about eight hours. The mixture was concentrated and the residue was purified by preparative TLC (5% methanol in dichloromethane) to afford the title compound (4.7 mg) as a white solid. MS (APCl+) Calc: 353.2, found: 354.2 (M+1).
WORKUP
后处理
- temperatureto reflux for about eight hours
- concentrationThe mixture was concentrated
- customthe residue was purified by preparative TLC (5% methanol in dichloromethane)