tert-Butyl piperazine-1-carboxylate → HCID 23081901, compound

HRID 1792039Notes

Reaction equation

HRID 1792039 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])[NH:7][C:6](=[O:19])[N:5]([CH3:20])[C:4]=2[N:3]=1.[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22]>C(OCC)(=O)C>[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][N:31]([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])[NH:7][C:6](=[O:19])[N:5]([CH3:20])[C:4]=3[N:3]=2)[CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:22])[CH3:23]

Participants

4

Reactant 2

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 22029591HCID 22029591, compound

Product 1

HCID 23081901HCID 23081901, compoundYield 51.2%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
150 °C

Procedure

8-Chloro-7-(2-chlorophenyl)-3-methyl-3,7-dihydropurine-2,6-dione (58 mg) and 1-(tert-butoxycarbonyl)piperazine (150 mg) were mixed. The reaction solution was stirred at 150° C. for 4 hours, then 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 chromatography to obtain 44 mg of the title compound from a fraction eluted with ethyl acetate.

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 chromatography

Sources & evidence

ORD record
ord-427692e7b0994aac9c5bce9e1eba85db
Source dataset
uspto-grants-2006_07
Patent number
US07074798B2

Reaction notes

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