Hydrochloric Acid → HCID 68577025, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:13][N:12]([CH2:14][CH:15]=[CH2:16])[CH2:11][CH2:10][N:9]2[CH2:17][CH:18]=[CH2:19])=[CH:4][CH:3]=1.[ClH:20].C(O)(C)C>C1(C)C=CC=CC=1>[ClH:1].[ClH:20].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C@@H:8]2[CH2:13][N:12]([CH2:14][CH:15]=[CH2:16])[CH2:11][CH2:10][N:9]2[CH2:17][CH:18]=[CH2:19])=[CH:6][CH:7]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 25 °C
Procedure
In toluene (5 mL), (R)-2-(4-Chlorophenyl)-1,4-di(2-propenyl)hexahydropyrazine (613 mg, 2.2 mmol) produced in Example 22 was dissolved. To the solution, 28 wt % hydrogen chloride solution in isopropanol (615 mg, 2.2 equivalents) was added, to precipitate crystals. The mixture was stirred at 25° C. for 1 hour. The crystals were separated by filtration under reduced pressure, washed with toluene (5 mL) and dried under vacuum, to obtain 643 mg of the title compound as white crystals (yield: 93%, chemical purity: 92.7 area %). The retention time in the chemical purity analysis method was 7.4 min.
Workup
- customto precipitate crystals
- customThe crystals were separated by filtration under reduced pressure
- washwashed with toluene (5 mL)
- customdried under vacuum
Sources & evidence
- ORD record
- ord-6c4a8053e21e4043bcf52234084a05fe
- Source dataset
- uspto-grants-2012_09
- Patent number
- US08273883B2
Reaction notes
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