HCID 18377306, compound → HCID 18377295, compound

HRID 2301096Notes

Reaction equation

HRID 2301096 reaction equation
[ClH:1].CO.C(OC([N:14]1[CH2:33][CH2:32][N:17]2[C:18]3[C:23]([N:24]([C:26](=[O:31])[C:27]([F:30])([F:29])[F:28])[CH2:25][CH:16]2[CH2:15]1)=[CH:22][CH:21]=[CH:20][CH:19]=3)=O)C1C=CC=CC=1>[Pd].C(O)C>[ClH:1].[F:30][C:27]([F:28])([F:29])[C:26]([N:24]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[N:17]2[CH2:32][CH2:33][NH:14][CH2:15][CH:16]2[CH2:25]1)=[O:31]

Participants

5

Reactant 2

HCID 18377306HCID 18377306, compoundHCID 21893726Hydrochloride methanol

Product 1

HCID 18377295HCID 18377295, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

A 80 μl portion of hydrochloric acid-methanol and 0.1 g of 10% Pd-C were added to 3 ml of ethanol solution containing 93 mg (0.22 mmol) of 3-benzyloxycarbonyl-2,3,4,4a,5,6-hexahydro-6-trifluoroacetyl-1H-pyrazino[1,2-a]quinoxaline, and 3 hours of catalytic hydrogenation was carried out at room temperature. The catalyst was filtered, the solvent was removed by evaporation under a reduced pressure and then the resulting residue was recrystallized from methanol-isopropyl ether to obtain 43 mg (61% in yield) of the title compound.

Workup

  1. customwas carried out at room temperature
  2. filtrationThe catalyst was filtered
  3. customthe solvent was removed by evaporation under a reduced pressure
  4. customthe resulting residue was recrystallized from methanol-isopropyl ether
  5. customto obtain

Sources & evidence

ORD record
ord-d9ab36e5894f4e96a2551a41a2a4da5b
Source dataset
uspto-grants-2002_12
Patent number
US06498251B1

Reaction notes

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