Dichloromethane → HCID 67119918, compound

Participants

Reaction Conditions

Reaction Steps

N-(1-(4-(1-pyrrolidinyl)phenyl)ethyl)-4-benzoylmethyl-4-piperidinol (III-25) is firstly prepared according to the method of synthesis and post-treatment in Example 2. 1.57 g (4.0 mmol) of N-(1-(4-(1-pyrrolidinyl) phenyl)ethyl)-4-benzoylmethyl-4-piperidinol is dissolved into 20 ml of anhydrous dichloromethane and cooled with dry ice-acetone with temperature controlled at below <−70° C. The reaction solution is added dropwise a dichloromethane solution (8 mol, 25 ml) of DAST under protecting of nitrogen gas. After completion of addition, the temperature is maintained at −75° C. and reacting for 1 hour, and the temperature is raised slowly and maintained at −10° C. and reacting for 2 hours. Then operating according to the post-treatment method in General Method six obtains 0.78 g of a white crystal, with yield of 40.2%.

Provenance & Evidence