HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl piperazine-1-carboxylate → HCID 67460900, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | HCID 86675326 | HCID 86675326 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 67460900 | HCID 67460900 | 44% |
Reaction Steps
To a solution of 4-chloro-5-ethyl-5,7-dihydrothieno[3,4-d]pyrimidine (0.3 g, 1.5 mmol) in n-BuOH (30 mL) was added 1-Boc-piperazine (0.8 g, 4.3 mmol), and the mixture was refluxed for 30 hours. The solvent was removed and the residue was purified by silica gel chromatography, eluting with Hexane/ethyl acetate (4:1-1:1) to give tert-butyl 4-(5-ethyl-5,7-dihydrothieno[3,4-d]pyrimidin-4-yl)piperazine-1-carboxylate (0.23 g, 44%). 1H NMR (CDCl3, 400 MHz) δ 8.54 (s, 1H), 4.61 (d, J=8.8 Hz, 1H), 4.10 (m, 2H), 3.80-3.60 (m, 8H), 2.02 (m, 1H), 1.60 (m, 1H), 1.49 (s, 9H), 0.95 (m, 3H). MS (APCI+) [M+H]+ 351.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09303040B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-5ebc32c02e8745068681b005c2a06bae |
| Source note | uspto-grants-2016_04 |