HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 89662793, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 7H-Pyrrolo[3′,4′:3,4]pyrazolo[1,5-a]pyrimidine-8(9H)-carboxylic acid, 3-chloro-2-methyl-, 1,1-dimethylethyl ester | HCID 89649693 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89662793 | HCID 89662793 | 78.3% |
Reaction Steps
A 32% solution of HCl (1.79 mL) was added to a solution of 6-chloro-5-methyl-1H,3H-2,4,7a,8-tetraaza-cyclopenta[a]indene-2-carboxylic acid tert-butyl ester (1.70 g; 5.51 mmol; 1 eq.) in AcOH (5.8 mL) and the reaction mixture was stirred at room temperature for 16 hours. The solution was diluted with DCM, washed with 1M NaOH (2×), dried over sodium sulfate and concentrated in vacuo to afford the title compound (900 mg, 78%) as a yellow solid. 1H NMR (DMSO-d6) δ 9.37 (s, 1H), 4.09-3.98 (m, 4H), 3.70-3.53 (m, 1M), 2.55 (s, 3H). HPLC (max plot) 99.8%, Rt 1.20 min. UPLC/MS: (MS+) 209.1 ([M+H]+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403835B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-a393b62ad14c49ba9d459633b913a80f |
| Source note | uspto-grants-2016_08 |