HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 6-Chloropyrimidine-2,4,5-triamine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2,5-Diamino-4,6-dichloropyrimidine | HCID 301039 | — |
| Reactant | 2-(6-fluoro-1H-benzo[d]imidazol-1-yl)-6-(piperidine-1-carbonyl)-9-(tetrahydro-2H-pyran-4-yl)-7H-purin-8(9H)-one | HCID 57612702 | — |
| Solvent | Water | HCID 962 | — |
| Product | 6-Chloropyrimidine-2,4,5-triamine hydrochloride | HCID 45789836 | 87% |
Reaction Steps
6-chloropyrimidine-2,4,5-triamine hydrochloride was prepared as described in WO 94/07892. 2,5-Diamino-4,6-dichloropyrimidine (10.8 g, 60.3 mmol) and concentrated aqueous ammonia (30 mL) were heated together in a sealed tube at 105° C. for 18 h, then cooled to room temperature. 2.34 g NaOH in water (10 mL) was added and the excess ammonia stripped out by concentrating to a low volume. Dilute HCl 2N (35 mL) and water (10 mL) were added and heated to dissolve, cooled to crystallize, then filtered to give the desired 6-chloropyrimidine-2,4,5-triamine hydrochloride (87% yield). MS (EI) m/z 160.1 (MH)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07919490B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-87bbf9fb5fc54a2e95d629648571c037 |
| Source note | uspto-grants-2011_04 |