HRID848428

反应详情

EQUATION

反应方程式

HRID 848428 的结构方程式

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

α,α-Diphenyl-α-(1-isopropyl-3-azetidinyl)acetonitrile (142 g.; 0.49 mole) was added to 500 g. of 70% sulfuric acid at 90°-100° C. The temperature was raised to 130° C. for 48 hours. The cooled mixture was poured onto ice and the cold mixture made basic by the addition of solid sodium hydroxide. The basic mixture was extracted with chloroform and the combined chloroform extracts dried over sodium sulfate and concentrated. The residual material was crystallized from an 80% isooctane- 20% isopropyl ether solution. The 4,5-dihydro-3,3-diphenyl-4-isopropylaminomethylfuran-2(3H)one weighed 105 g. (69.3%) and melted at 78°-80° C.

WORKUP

后处理

  1. customat 90°-100° C
  2. additionThe cooled mixture was poured onto ice
  3. extractionThe basic mixture was extracted with chloroform
  4. dry with materialthe combined chloroform extracts dried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residual material was crystallized from an 80% isooctane- 20% isopropyl ether solution