Hydrochloric Acid → HCID 68577025, compound

HRID 2390916Notes

Reaction equation

HRID 2390916 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]=1

Participants

5

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

  1. customto precipitate crystals
  2. customThe crystals were separated by filtration under reduced pressure
  3. washwashed with toluene (5 mL)
  4. customdried under vacuum

Sources & evidence

ORD record
ord-6c4a8053e21e4043bcf52234084a05fe
Source dataset
uspto-grants-2012_09
Patent number
US08273883B2

Reaction notes

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