HRID488098

反应详情

EQUATION

反应方程式

HRID 488098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In an Erlenmeyer flask, 1.35 g of para-aminobenzoic acid chloride are dissolved in 20 ml benzene in the presence of 2.8 ml triethylamine. 1.49 g L-methionine is added progressively and the resultant mixture is filtered. After evaporation of the filtrate to dryness under vacuum (15 mm Hg), the residue is dissolved in N hydrochloric acid and extracted with chloroform. The chloroformic solution is successively washed with several ml of 10% aqueous HKCO3 solution and with water. It is then collected, dried over magnesium sulfate and evaporated. The product obtained is precipitated in cyclohexane and filtered. After recrystallization in a (1:1) mixture of 95 alcohol-water, 1.95 g of white crystals are isolated. M.p.: 172° C.

WORKUP

后处理

  1. filtrationthe resultant mixture is filtered
  2. customAfter evaporation of the filtrate to dryness under vacuum (15 mm Hg)
  3. dissolutionthe residue is dissolved in N hydrochloric acid
  4. extractionextracted with chloroform
  5. washThe chloroformic solution is successively washed with several ml of 10% aqueous HKCO3 solution and with water
  6. customIt is then collected
  7. dry with materialdried over magnesium sulfate
  8. customevaporated
  9. customThe product obtained
  10. customis precipitated in cyclohexane
  11. filtrationfiltered
  12. customAfter recrystallization
  13. additionin a (1:1) mixture of 95 alcohol-water, 1.95 g of white crystals
  14. customare isolated