HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 2-Chloro-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 2,6-Dichloro-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purine | HCID 57699703 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 2-Chloro-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine | HCID 57699804 | — |
Reaction Steps
2,6-dichloro-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purine (3.08 g, containing triphenylphosphine oxide) was heated with 2M ammonia in IPA (50 mL) at 50° C., overnight. The reaction mixture was then evaporated to dryness to give a yellow solid. This material (3.2089 g) was recrystallised using methanol (50 mL) and after cooling the resultant solid was filtered and washed with methanol (5 mL) to give the title compound (1.5554 g). The filtrate was evaporated and recrystallised from methanol (25 mL) and after cooling the resultant solid was filtered to give a second crop (0.2324 g) and was consistent with first batch by NMR and LCMS.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977344B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-bad6482d8b25469683fd20bb289c6f78 |
| Source note | uspto-grants-2011_07 |