HRID2184099

反应详情

EQUATION

反应方程式

HRID 2184099 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Phenyl-1,2,3,4-tetrahydropyridine hydrochloride (15.92 mg, 0.10 mmol) was suspended in methylene chloride (2 ml). Ethyldiisopropylamine (0.035 ml, 0.20 mmol) was added and the solution was shaken for 10 minutes at room temperature. 2,2-Diphenyl-benzo[1,3]dioxole-5-sulfonyl chloride (37.28 mg, 0.10 mmol) was added and the reaction was shaken at room temperature for 12 hours. Aqueous HCl (0.1 N, 1.0 ml) was added and the mixture shaken for 30 minutes, the aqueous layer removed and the organic phase concentrated and purified by preparative reverse phase HPLC (YMC, ODS-AQ packing; 20%→95% CH3CN/H2O) to yield the sulfonamide (23.6 mg, 48%).

WORKUP

后处理

  1. stirringthe reaction was shaken at room temperature for 12 hours
  2. stirringthe mixture shaken for 30 minutes
  3. customthe aqueous layer removed
  4. concentrationthe organic phase concentrated
  5. custompurified by preparative reverse phase HPLC (YMC, ODS-AQ packing; 20%→95% CH3CN/H2O)