反应详情

Step 2): SOCl2 (0.6 ml, 8.2 mmol) was added dropwise to a solution of 1-diphenylmethyl-4-hydroxymethylpiperidine (1.0 g, 3.6 mmol) in benzene (7 ml) at room temperature. The mixture was refluxed for 18 hours and then concentrated. The residue was dissolved in ethyl acetate, washed with 5% NaOH solution, dried (MgSO4) and concentrated. The residue was recrystallized (ethyl acetate/ether/hexane) to give 1-diphenylmethyl-4-chloromethylpiperidine (70.1%): mp 73°-75° C.

1. temperatureThe mixture was refluxed for 18 hours
2. concentrationconcentrated
3. dissolutionThe residue was dissolved in ethyl acetate
4. washwashed with 5% NaOH solution
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customThe residue was recrystallized (ethyl acetate/ether/hexane)