HRID906219

反应详情

EQUATION

反应方程式

HRID 906219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

To an ice-cold solution of 5-hydroxymethyl-1-(toluene-4-sulfonyl)-pyrrolidin-3-ol (4) (0.45 g, 1.66 mmol) in pyridine (3 mL) is added 4-toluylsulfonyl chloride (1.11 g, 5.81 mmol) in one portion. The temperature rises to 50° C., then the reaction mixture is cooled to 10° C., kept at that temperature for an additional 2 h and then left at room temperature overnight. The mixture is poured into 2N HCl (13 mL). On cooling the compound precipitates out and separated by filtration, washed with cold water (2×5 mL), and dried under reduced pressure to give compound (5) as white solid.

WORKUP

后处理

  1. customrises to 50° C.
  2. waitleft at room temperature overnight
  3. temperatureOn cooling the compound
  4. customprecipitates out and
  5. customseparated by filtration
  6. washwashed with cold water (2×5 mL)
  7. customdried under reduced pressure