HCID 89924447, compound → 1226160-70-8

HRID 2200353Notes

Reaction equation

HRID 2200353 reaction equation
C([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)[CH2:10][C:9]1([CH3:22])[CH3:21])C1C=CC=CC=1>CO.C(OCC)(=O)C.[Pd]>[F:20][C:17]1[CH:16]=[CH:15][C:14]([N:11]2[CH2:12][CH2:13][NH:8][C:9]([CH3:22])([CH3:21])[CH2:10]2)=[CH:19][CH:18]=1

Participants

5

Reactant 1

HCID 89924447HCID 89924447, compound

Product 1

HCID 572767191226160-70-8

Reagents, catalysts & solvents 3

HCID 23938PalladiumCatalystHCID 887MethanolSolventHCID 8857Ethyl AcetateSolvent

Conditions

Temperature
50 °C

Procedure

To a stirred solution of 1-benzyl-4-(4-fluorophenyl)-2,2-dimethylpiperazine (4.5 g, 15.08 mmol) in methanol and ethyl acetate (5:1, 60 ml) at 25° C. was added 10% palladium on charcoal (1.605 g). The reaction mixture was stirred at 50° C. for 5 h. The progress of reaction was monitored by TLC. The reaction mixture was cooled to room temperature, filtered through a celite bed, washed with ethyl acetate (2×50 ml). The combined filtrate was concentrated under reduced pressure to obtain the title compound which was used in the next step without further purification.

Workup

  1. customThe progress of reaction
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationfiltered through a celite bed
  4. washwashed with ethyl acetate (2×50 ml)
  5. concentrationThe combined filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-cddfff64cb2a4d51a3df076ec01decaa
Source dataset
uspto-grants-2016_06
Patent number
US09359367B2

Reaction notes

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