A kind of synthetic method of α,α-diphenyl-4-piperidinemethanol
A technology of piperidine methanol and synthesis method, applied in directions such as organic chemistry, can solve the problem of high production cost, achieve the effects of low production cost, easy operation and suitability for industrialization
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0030] A kind of α, the synthetic method of α-diphenyl-4-piperidinemethanol, the concrete steps of its synthetic process are as follows:
[0031] (1) Synthesis of N-acetyl-4-piperidinecarboxylic acid
[0032] Add 4-piperidinecarboxylic acid (38.8g, 0.30mol) and 58mL of acetic anhydride to a 250mL four-neck flask equipped with a drying tube at the mouth of the condenser, slowly raise the temperature to reflux and continue for 6h, TLC detects that the reaction is complete, and the obtained The reaction solution was cooled to room temperature, a large amount of light brown solid precipitated out, the solid was filtered out with suction, the solid was washed with an appropriate amount of methyl tert-butyl ether and then filtered with suction to obtain a light brown solid, which was recrystallized with methanol to obtain 46.3 g of an off-white solid, which was collected Rate 90.1%;
[0033] The amount of 4-piperidinecarboxylic acid and acetylating reagent used in the above N-acety...
Embodiment 2
[0050] A kind of α, the synthetic method of α-diphenyl-4-piperidinemethanol, the concrete steps of its synthetic process are as follows:
[0051] (1) Add 4-piperidinecarboxylic acid (38.8g, 0.30mol) and 32mL acetyl chloride into a 250mL four-neck flask equipped with a drying tube at the mouth of the condenser, slowly raise the temperature to reflux and continue for 4h, then detect the reaction by TLC After completion, the resulting reaction solution was cooled to room temperature, a large amount of light brown solid precipitated, the solid was filtered out with suction, the solid was washed with an appropriate amount of methyl tert-butyl ether and then filtered with suction to obtain a light brown solid, which was recrystallized with methanol to obtain an off-white solid 46.3g, yield 90.1%;
[0052] The amount of 4-piperidinecarboxylic acid and acetylating reagent used in the above N-acetylation reaction is calculated in molar ratio, that is, 4-piperidinecarboxylic acid: acety...
PUM
| Property | Measurement | Unit |
|---|---|---|
| melting point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More