HRID2275338

反应详情

EQUATION

反应方程式

HRID 2275338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(2R,4R)-tert-Butyl 2-(3-fluorophenyl)-4-hydroxypyrrolidine-1-carboxylate (1.4 g, 4.98 mmol) and Dess-Martin periodinane (2.53 g, 5.97 mmol) were mixed in 50 mL DCM and stirred at ambient temperature overnight. For workup, 20 mL 1N NaOH was added to reaction, and stirred for 30 minutes, followed by addition of 20 mL brine. The reaction mixture was extracted with several portions of DCM. The combined organic extracts were filtered through a Phase Separator filter paper, concentrated, and purified by reverse phase chromatography, eluting with 20-70% acetonitrile/water to yield the product as yellow oil (600 mg, 43% yield.)

WORKUP

后处理

  1. stirringstirred for 30 minutes
  2. extractionThe reaction mixture was extracted with several portions of DCM
  3. filtrationThe combined organic extracts were filtered through a Phase Separator
  4. filtrationfilter paper
  5. concentrationconcentrated
  6. custompurified by reverse phase chromatography
  7. washeluting with 20-70% acetonitrile/water