反应详情

温度

70 °C

To 80 ml. of concentrated sulfuric acid preheated to 70° C. was added 25 g. (0.86 mole) of α-(1-isopropyl-3-azetidinyl)-α,α-diphenylacetonitrile at a rate to maintain a temperature of 65°-75° C. The solution was heated at 70° C. for 18 hrs. and poured on ice. The mixture was made basic with 50% sodium hydroxide (while cooling with ice) and extracted with chloroform. The chloroform was dried (sodium sulfate) and concentrated. The residue was crystallized from ethyl acetate-ethanol to give 15.7 g. (59%) of product melting at 181°-184° C.

1. custompreheated to 70° C.
2. additionwas added 25 g
3. additionand poured on ice
4. extractionextracted with chloroform
5. dry with materialThe chloroform was dried (sodium sulfate)
6. concentrationconcentrated
7. customThe residue was crystallized from ethyl acetate-ethanol
8. customto give 15.7 g