HRID967349

反应详情

EQUATION

反应方程式

HRID 967349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirrer, a thermometer and a dropping funnel were set to a 1,000-mL four-necked flask and to a reaction apparatus, 95% sulfuric acid (450 g, 4.4 mol) was added and cooled so that the liquid temperature was lower than 30° C. To the cooled sulfuric acid with stirring, was added α-n-butyl-α-hydroxyacetonitrile prepared from n-butyl aldehyde and hydrocyanic acid (1.5 mol, content 87 to 94%, further containing unreacted hydrocyanic acid, starting material n-butyl aldehyde and water) with the use of dropping funnel. The addition was conducted in such a way that the reaction solution was kept at a temperature of lower than 40° C. After the dropwise addition, the reaction solution was aged at 40° C. for 0.5 hr. The pH of the reaction solution was less than 1. A part of the reaction solution was sampled and analyzed by HPLC. In result, the ratio of conversion of the starting materials was 100% and the corresponding 2-hydroxyhexanoic acid amide and 2-hydroxysulfonyl oxy hexanoic acid amide were produced.

WORKUP

后处理

  1. additionwas added
  2. temperaturecooled so that the liquid temperature
  3. customwas lower than 30° C
  4. additionThe addition
  5. customlower than 40° C
  6. additionAfter the dropwise addition
  7. aliquotA part of the reaction solution was sampled
  8. customIn result