HCID 20141227, compound → HCID 20141228, compound

HRID 570003Notes

Reaction equation

HRID 570003 reaction equation
[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[N:11][C:12]([N:14]3[CH2:19][CH2:18][N:17](CC4C=CC=CC=4)[CH2:16][CH2:15]3)=[N:13][C:6]=2[CH:5]([CH3:27])[CH2:4][NH:3]1>C(O)C.[Pd]>[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[N:11][C:12]([N:14]3[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]3)=[N:13][C:6]=2[CH:5]([CH3:27])[CH2:4][NH:3]1

Participants

4

Reactant 1

HCID 20141227HCID 20141227, compound

Product 1

HCID 20141228HCID 20141228, compoundYield 67%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

Dissolved in 10 ml of ethanol was 0.2 g (0.55 mmol) of 6,9-dimethyl-2-(4-benzylpiperazino)-5-oxo-5,6,7,8-tetrahydro(9H)pyrimido[4,5-e]diazepine, followed by an addition of 20 mg of 10% Pd-C. Under reflux, the reactant was hydrogenated at atmospheric pressure for 2 hours. After cooling the reaction mixture to room temperature, the catalyst was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography to obtain 0.1 g of the intended product (yield: 67%).

Workup

  1. temperatureUnder reflux
  2. filtrationthe catalyst was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by column chromatography

Sources & evidence

ORD record
ord-5365d6dbfe0746579f51d7f8c6ef2ed4
Source dataset
uspto-grants-1988_03
Patent number
US04734418

Reaction notes

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