HRID965335

反应详情

EQUATION

反应方程式

HRID 965335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 3-aminopropionate hydrochloride (10 g) was dissolved in a mixture of tetrahydrofuran (100 ml) and water, which was cooled at 0° to 5° C. in an ice bath and adjusted to pH 8.2 with 30% aqueous sodium hydroxide solution. To a resulting solution was added with care benzyloxycarbonyl chloride (10.3 ml), with maintaining the pH from pH 8.0 to 9.0 with 30% aqueous sodium hydroxide solution at 0° to 5° C. The reaction mixture was extracted with ethyl acetate (300 ml) and organic layer was separated, which was washed two times with saturated sodium chloride in water and dried over magnesium sulfate. Solvent was removed under reduced pressure to give ethyl 3-(benzyloxycarbonylamino)-propionate (15.3 g).

WORKUP

后处理

  1. temperaturewas cooled at 0° to 5° C. in an ice bath
  2. extractionThe reaction mixture was extracted with ethyl acetate (300 ml) and organic layer
  3. customwas separated
  4. washwhich was washed two times with saturated sodium chloride in water
  5. dry with materialdried over magnesium sulfate
  6. customSolvent was removed under reduced pressure