tert-Butyl piperazine-1-carboxylate → HCID 23536931, compound

HRID 1792081Notes

Reaction equation

Cl[C:2]1[N:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH:17]=[O:18])[C:9]2[C:8](=[O:19])[N:7]([CH2:20][O:21][C:22](=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24])[C:6](=[O:28])[N:5]([CH2:29][O:30][C:31](=[O:36])[C:32]([CH3:35])([CH3:34])[CH3:33])[C:4]=2[N:3]=1.[C:37]([O:41][C:42]([N:44]1[CH2:49][CH2:48][NH:47][CH2:46][CH2:45]1)=[O:43])([CH3:40])([CH3:39])[CH3:38]>C(Cl)(Cl)Cl>[C:37]([O:41][C:42]([N:44]1[CH2:49][CH2:48][N:47]([C:2]2[N:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:17]=[O:18])[C:9]3[C:8](=[O:19])[N:7]([CH2:20][O:21][C:22](=[O:27])[C:23]([CH3:24])([CH3:26])[CH3:25])[C:6](=[O:28])[N:5]([CH2:29][O:30][C:31](=[O:36])[C:32]([CH3:35])([CH3:34])[CH3:33])[C:4]=3[N:3]=2)[CH2:46][CH2:45]1)=[O:43])([CH3:40])([CH3:38])[CH3:39]

Participants

Conditions

Temperature: 150 °C

Procedure

2,2-Dimethylpropionic acid [8-chloro-1-(2,2-dimethyl-propionyloxymethyl)-7-(2-formylphenyl)-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl ester (2.0 g) and piperazine-1-carboxylic acid tert-butyl ester (2.15 g) were mixed, and the mixture was stirred at 150° C. for 1 hour and 10 minutes. The reaction mixture was diluted with chloroform and purified by silica gel column chromatography to give 1.94 g of the title compound from the elution fraction of hexane-ethyl acetate (1:1).

Workup

custompurified by silica gel column chromatography

Sources & evidence

ORD record: ord-15d6af6873dd481bba186ab0b176bf15
Source dataset: uspto-grants-2006_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07074798B2

Reaction notes

Loading…