HRID1662042

反应详情

EQUATION

反应方程式

HRID 1662042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of (1S,2R)-2-[(tert-butoxycarbonyl)amino]cyclopentanecarboxylic acid (0.88 g) and DMF (8.0 ml) were added cesium carbonate (2.5 g) and methyl iodide (0.82 g) under ice-cooling, followed by stirring at room temperature for 1.5 hours. To the reaction mixture ethyl acetate and water under ice-cooling were added. The organic layer was separated, the aqueous layer was extracted with ethyl acetate (15 ml), and the organic layer was combined and washed with a 10% aqueous citric acid solution, a saturated sodium bicarbonate solution, water, and saturated brine in this order. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain methyl (1S,2R)-2-[(tert-butoxycarbonyl)amino]cyclopentanecarboxylate (0.85 g).

WORKUP

后处理

  1. temperaturecooling
  2. additionwere added
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with ethyl acetate (15 ml)
  5. washwashed with a 10% aqueous citric acid solution
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure