HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 58299854, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | tert-Butyl 4-(6-((9-cyclopentyl-8-methyl-7-oxo-8,9-dihydro-7H-pyrido[3',2':4,5]-pyrrolo[2,3-d]pyrimidin-2-yl)amino)-3-pyridinyl)-1-piperazinecarboxylate | HCID 58299974 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58299854 | HCID 58299854 | 62.5% |
Reaction Steps
Compound 274 (51 mg) was dissolved in 2 mL dioxane. Dioxane (1 mL) saturated at room temperature with HCl was added, followed by 1 mL methanol to aid solution. The reaction was stirred at room temperature for 80 min. The solution was then added dropwise to diethyl ether (8 mL) and the resulting precipitate was collected and dried in vacuo to give compound 271 as a yellow solid (26 mg, 62%). 1H NMR (500 MHz, DMSO-d6) δ 11.75 (br. s., 1 H) 9.36 (br. s., 2 H) 9.20 (s, 1 H) 8.53 (d, J=8.31 Hz, 1 H) 7.91-8.01 (m, 2 H) 7.49 (d, J=9.29 Hz, 1 H) 6.83 (d, J=8.56 Hz, 1 H) 5.37 (quin, J=8.56 Hz, 1 H) 3.35-3.43 (m, 5 H) 1.94-2.13 (m, 4 H) 1.64-1.79 (m, 2 H) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841312B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-95475c638f2640dd990b93f9612f4d9d |
| Source note | uspto-grants-2014_09 |