HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178503438, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N,N-Dimethylethylenediamine | HCID 66053 | — |
| Reactant | HCID 178503430 | HCID 178503430 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 178503438 | HCID 178503438 | 75.3% |
Reaction Steps
To a solution of 6-chloro-3-(2-methylsulfanyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidine (from Example 7 supra) (400 mg, 1.43 mmol) in 2-propanol (40 mL) was added N, N-dimethylethane-1,2-diamine (139 mg, 1.58 mmol) followed by triethylamine (159 mg, 1.57 mmol). The reaction mixture was stirred at reflux for 15 hours and the solvent was then removed under reduced pressure. The residue was extracted with dichloromethane (3×30 mL), washed with water (5 mL), dried over anhydrous sodium sulfate, filtered, and concentrated to afford N,N-dimethyl-N′-[3-(2-methylsulfanyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-ethane-1,2-diamine (Yield 356 mg, 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362023B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-054f093b3b7b44ee84de12be77728e61 |
| Source note | uspto-grants-2013_01 |