HRID224597

反应详情

EQUATION

反应方程式

HRID 224597 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

155 g of L-histidine and 189 g of sodium hydrogen carbonate were dissolved in 1 liter of water and 124 g of chloroacetyl chloride was added dropwise to the resulting solution with stirring and ice-cooling. After allowing the reaction to proceed for 1 hour, an aqueous solution of sodium thiobenzoate which was prepared from 152 g of thiobenzoic acid and 220 ml of 5 N solution of sodium hydroxide solution, was added dropwise to the resulting solution and was kept standing overnight at room temperature to allow reaction. The resulting reation solution was acidified with hydrochloric acid with ice-cooling to precipitate crystals. The crystals were collected on the filter and washed with water. The product thus obtained weighed 140 g (42 percent of the theoretical amount). Recrystallization from water gave colorless needles, m.p. 176°-177° C.

WORKUP

后处理

  1. temperatureice-cooling
  2. customthe reaction
  3. additionwas added dropwise to the resulting solution
  4. waitwas kept standing overnight at room temperature
  5. customreaction
  6. temperaturecooling
  7. customto precipitate crystals
  8. customThe crystals were collected on the
  9. filtrationfilter
  10. washwashed with water
  11. customThe product thus obtained
  12. customRecrystallization from water
  13. customgave colorless needles, m.p. 176°-177° C.