tert-Butyl piperazine-1-carboxylate → HCID 23081912, compound

HRID 1792030Notes

Reaction equation

HRID 1792030 reaction equation
Cl[C:2]1[N:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])[C:9]2[C:8](=[O:18])[N:7]([CH3:19])[C:6](=[O:20])[N:5]([CH3:21])[C:4]=2[N:3]=1.[C:22]([O:26][C:27]([N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1)=[O:28])([CH3:25])([CH3:24])[CH3:23]>C(OCC)(=O)C>[C:22]([O:26][C:27]([N:29]1[CH2:34][CH2:33][N:32]([C:2]2[N:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:9]3[C:8](=[O:18])[N:7]([CH3:19])[C:6](=[O:20])[N:5]([CH3:21])[C:4]=3[N:3]=2)[CH2:31][CH2:30]1)=[O:28])([CH3:25])([CH3:23])[CH3:24]

Participants

4

Reactant 2

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 30557721H-Purine-2,6-dione, 3,7-dihydro-8-chloro-7-(2-chlorophenyl)-1,3-dimethyl-

Product 1

HCID 23081912HCID 23081912, compoundYield 68.9%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
150 °C

Procedure

8-Chloro-7-(2-chlorophenyl)-1,3-dimethyl-3,7-dihydropurine-2,6-dione (142 mg) and piperazine-1-carboxylic acid tert-butyl ester (500 mg) were mixed, and the reaction mixture was stirred at 150° C. for 4 hours, diluted with ethyl acetate, and washed with water. The organic layer was dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 143 mg of the title compound from a fraction eluted with hexane-ethyl acetate (2:3).

Workup

  1. washwashed with water
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography

Sources & evidence

ORD record
ord-1136e65f66bf452d8e71c88c0c626771
Source dataset
uspto-grants-2006_07
Patent number
US07074798B2

Reaction notes

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