Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-tert-Butyl 3-ethyl piperazine-1,3-dicarboxylate | HCID 11402671 | — |
| Reactant | 6-Chloro-8-(2-chlorophenyl)-9-(4-chlorophenyl)-9H-purine | HCID 21905779 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69364884 | HCID 69364884 | — |
Reaction Steps
6-Chloro-9-(4-chlorophenyl)-8-(2-chlorophenyl)-9H-purine I-(4A-7)c (103 mg, 0.27 mmol), piperazine-1,3-dicarboxylic acid 1-tert-butyl ester 3-ethyl ester (Chiu, C. K.-F. and Griffith, D. A., EP 1004583 A2; 156 mg, 0.60 mmol), and triethylamine (95 μl, 0.68 mmol) were combined in ethanol (1.5 ml) and heated at 60° C. until complete by TLC (3 days). The reaction mixture was concentrated under reduced pressure and then purified on a Biotage™ Flash 12M column using 20 to 30% ethyl acetate in hexanes as eluant to afford title compound I-(8A-1)a (78 mg, 48%): +ESI MS (M+1) 597.3; 1H NMR (400 MHz, CD3OD) δ 8.298 (br s, 1H), 7.57 (br s, 1H), 7.48–7.25 (m, 7H), 5.60 (v br s, 1H), 4.67 (d, J=13.7 Hz, 1H), 4.23–4.05 (br m, 3H), 3.43–3.00 (br m, 2H), 1.46 (s, 9H), 1.22 (t, J=7.1 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07129239B2 |
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| Source dataset | uspto-grants-2006_10 |
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| ORD ID | ord-ea1029e404fb4b44a43f1ac32f02a15d |
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| Source note | uspto-grants-2006_10 |
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