HRID1671746

反应详情

EQUATION

反应方程式

HRID 1671746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

294 g (2.51 mol) of L-valine was dissolved into 786 g of ion-exchange water, 358 g (2.42 mol) of an aqueous solution of 27% sodium hydroxide and 363 g of acetone. With stirring the solution, 533 g (2.43 mol) of lauroyl chloride and 358 g (2.47 mol) of an aqueous solution of 27% sodium hydroxide were simultaneously added dropwise thereto so that pH=12±0.2 and the temperature is kept at 19 to 20° C. After completion of the addition, the solution was stirred at 20° C. for 60 minutes. Then, it was heated up to 40° C., and 171 g of 75% sulfuric acid was added thereto in order to adjust pH=1.5. The layers of the oily substance and water phase that separated at 60° C. were split, and 1950 g of warm water of 60° C. was added to the oily substance. After the mixture was cooled down to 20° C., the precipitated solid substance was filtered out and washed with water. Then, the substance was vacuum-dried at 50° C. to obtain 710 g of N-lauroyl-L-valine (2.37 mol, yield 98%).

WORKUP

后处理

  1. additionwere simultaneously added dropwise
  2. customis kept at 19 to 20° C
  3. additionAfter completion of the addition
  4. temperatureThen, it was heated up to 40° C.
  5. customThe layers of the oily substance and water phase that separated at 60° C.
  6. customwere split
  7. addition1950 g of warm water of 60° C. was added to the oily substance
  8. temperatureAfter the mixture was cooled down to 20° C.
  9. filtrationthe precipitated solid substance was filtered out
  10. washwashed with water
  11. customThen, the substance was vacuum-dried at 50° C.