HRID2038582

反应详情

EQUATION

反应方程式

HRID 2038582 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

L-Phenylalanine was converted to 4-nitro-L-phenylalanine by a conventional nitration process known in the art. Thereafter, about 100 g of 4-nitro-L-phenylalanine was dissolved in about 600 mL of about 3.5% methanolic sodium hydroxyide solution and hydrogenated by hydrogen gas at a pressure of about 45 psi in the presence of a 5% palladium/carbon catalyst with the pH of the solution being about 11. The temperature of the reaction mixture was maintained from about 20° C. to about 40° C. The reaction mixture was periodically monitored for the completion of reaction by use of HPLC analysis. The reaction mixture was then filtered to remove the palladium/carbon catalyst and neutralized to about pH 7 with acetic acid. The neutralized filtrate was cooled to about 5° C., until 4-amino-L-phenylalanine precipitated out. The precipitate was isolated by filtration, washed with methanol and dried. (Weight 76 g, HPLC Purity 98%.)

WORKUP

后处理

  1. temperatureThe temperature of the reaction mixture was maintained from about 20° C. to about 40° C
  2. customThe reaction mixture was periodically monitored for the completion of reaction by use of HPLC analysis
  3. filtrationThe reaction mixture was then filtered
  4. customto remove the palladium/carbon catalyst
  5. customprecipitated out
  6. customThe precipitate was isolated by filtration
  7. washwashed with methanol
  8. customdried