Hydrogen Bromide → HCID 178419735, compound
Reaction equation
C[O:2][C:3]1[N:8]=[CH:7][C:6]([C:9]2([CH2:15][CH2:16][CH2:17]O)[CH2:14][CH2:13][CH2:12][NH:11][CH2:10]2)=[CH:5][CH:4]=1.[BrH:19]>>[BrH:19].[Br:19][CH2:17][CH2:16][CH2:15][C:9]1([C:6]2[CH:5]=[CH:4][C:3]([OH:2])=[N:8][CH:7]=2)[CH2:14][CH2:13][CH2:12][NH:11][CH2:10]1Participants
3
Conditions
- Temperature
- 110 °C
Procedure
0.100 g (0.4 mmol) of 3-[3-(6-methoxypyridin-3-yl)piperidin-3-yl]propan-1-ol obtained in stage 1.3, in solution in 5 ml of aqueous hydrobromic acid (48% by weight solution), is introduced into a sealed tube. The reaction medium is stirred at 110° C. for 12 hours. This solution is then brought back to ambient temperature and concentrated under reduced pressure. The resulting residue is dissolved in methanol and evaporated twice under reduced pressure, and triturated from diethyl ether, to result, after filtration, in 0.150 g of the desired compound in the form of a brown powder.
Workup
- customis then brought back to ambient temperature
- concentrationconcentrated under reduced pressure
- dissolutionThe resulting residue is dissolved in methanol
- customevaporated twice under reduced pressure
- customtriturated from diethyl ether
- customto result
- filtrationafter filtration
Sources & evidence
- ORD record
- ord-19bd27f98d9f4c01b151dc32c515fb43
- Source dataset
- uspto-grants-2014_06
- Patent number
- US08759343B2
Reaction notes
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