HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 178481615, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | 2-tert-butylimino-N,N-diethyl-1-methyl-1,3,2lambda5-diazaphosphinan-2-amine | HCID 19990018 | — |
| Reactant | HCID 178518645 | HCID 178518645 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178481615 | HCID 178481615 | — |
Reaction Steps
To a solution of 6-chloro-2-(6-fluoro-1H-benzo[d]imidazol-1-yl)-9-(trans-4-(tetrahydro-2H-pyran-2-yloxy)cyclohexyl)-7H-purin-8(9H)-one (0.06 mmol) in anhydrous CH3CN (10 mL) were added BEMP on polystyrene (loading 2.2 mmol/g, 4 equiv.) and iodomethane (primary alkyl iodide/benzyl iodide or bromide to be used for alkylation) (6 equiv.) with stirring at room temperature. After 1 h, LCMS showed reaction to be complete. The reaction mixture was filtered under vacuum, the resin washed with CH3CN and methanol, and the combined filtrate and washings were concentrated in vacuo to give the desired product as a pale yellow solid, which was used in the next step without further purification. MS (EI) m/z 501.2 (MH)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07902187B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-3e45e6692dc84ff6a90cb72ab3bd0698 |
| Source note | uspto-grants-2011_03 |