HRID463360

反应详情

EQUATION

反应方程式

HRID 463360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To 5.22 g (0.020 mol) of N-(1-cyano-1,2-dimethylpropyl)phthalamic acid in a mixture of 35 mL isopropyl alcohol and 10 mL of water is added 6.41 g (0.080 mol) of aqueous 50% sodium hydroxide. External cooling is applied to hold the temperature at 20°-30° C. and 4.80 g (0.042 mol) of aqueous 30% hydrogen peroxide is added. The mixture is heated at 80° C. for five hours then cooled to 20°-25° C. Aqueous 36% hydrochloric acid is added to adjust the pH to 1. The volatile solvent is removed in vacuo to give 8.35 g of solid 2-(5-isopropyl-5-methyl-4-oxo-2-imidazolin-2-yl)benzoic acid, hydrochloride salt. The solid is analyzed by high performance liquid chromatography. The real yield is 60.3%.

WORKUP

后处理

  1. temperatureExternal cooling
  2. customat 20°-30° C.
  3. temperaturethen cooled to 20°-25° C
  4. customThe volatile solvent is removed in vacuo