Acetic Anhydride → 1-(3-Hydroxypiperidin-1-yl)ethan-1-one
Reaction equation
[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3]1.[C:8](OC(=O)C)(=[O:10])[CH3:9]>C(Cl)Cl>[C:8]([N:4]1[CH2:5][CH2:6][CH2:7][CH:2]([OH:1])[CH2:3]1)(=[O:10])[CH3:9]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 10 °C
Procedure
3-Hydroxypiperidine (0.4 mole) is dissolved in 150 ml. of methylene chloride. The solution is cooled to 10° C. and acetic anhydride (0.46 mole) is added dropwise, maintaining the temperature under 20° C. The reaction mixture is allowed to come to room temperature, and is then refluxed for 2 hours. The methylene chloride is evaporated off, and the remaining liquid is distilled under high vacuum. A thick yellow oil is collected at 122°-126° C. (0.3 mm Hg).
Workup
- temperaturemaintaining the temperature under 20° C
- customto come to room temperature
- temperatureis then refluxed for 2 hours
- customThe methylene chloride is evaporated off
- distillationthe remaining liquid is distilled under high vacuum
- customA thick yellow oil is collected at 122°-126° C. (0.3 mm Hg)
Sources & evidence
- ORD record
- ord-0b73d369403e428bad7718ae4e2f4d7f
- Source dataset
- uspto-grants-1983_03
- Patent number
- US04377521
Reaction notes
Loading…