HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 17968223, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 17968209 | HCID 17968209 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 17968223 | HCID 17968223 | 34% |
Reaction Steps
To a solution of 7-(2,2-dimethyl-propyl)-6-(2,4-dioxo-3-propyl-1,3,8-triaza-spiro[4.5]dec-8-ylmethyl)-7H-pyrrolo[2,3-d]pyrimidine-2-carbonitrile (0.2 g, 0.48 mmol) in DMF (2 ml), NaH (22 mg, 0.55 mmol) and MeI (50 □1, 0.55 mmol) are added at 0° C. The reaction mixture is stirred at ambient temperature for 4 h, quenched with saturated ammonium chloride and extracted with AcOEt. The organic layer is washed with brine, dried over magnesium sulfate and filtrated The combined extracts are concentrated and the residue is purified by column chromatography on silica gel using CH2Cl2:MeOH=25:1 (v/v) and CH2Cl2:MeOH=15:1 (v/v) to give 71 mg of desired product in 34% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07452886B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-b59cca17a5634d998c8b2e20e1f7162a |
| Source note | uspto-grants-2008_11 |