HRID848845

反应详情

EQUATION

反应方程式

HRID 848845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

To a stirred mixture of p-hydroxymethylbenzaldehyde (10.0 g., 0.0735 mole) and ammonium carbonate (17.1 g., 0.15 mole) in 110 ml. of 60% ethanol heated to 50° C. there was added dropwise sodium cyanide (4.0 g., 0.081 mole) dissolved in 10 ml. water. The mixture was stirred and heated to 55°-60° C. for three hours and then the temperature raised to 85° C. for one hour. After cooling in an ice bath, the pH of the solution was brought to 6 by the addition of concentrated hydrochloric acid. Upon overnight cooling, the solid which had precipitated was filtered, washed with cold water, and dried. The 5-(p-hydroxymethylphenyl)hydantoin (11.0 g., 72% yield), m.p. 189°-196° (dec.), was used to prepare the amino acid without further purification.

WORKUP

后处理

  1. dissolutiondissolved in 10 ml
  2. temperatureheated to 55°-60° C. for three hours
  3. temperatureAfter cooling in an ice bath
  4. temperatureUpon overnight cooling
  5. customthe solid which had precipitated
  6. filtrationwas filtered
  7. washwashed with cold water
  8. customdried