HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 9984757, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 68981335 | HCID 68981335 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 9984757 | HCID 9984757 | 58% |
Reaction Steps
To a solution of 7-(2-cyclohexyl-ethyl)-6-(4-oxo-1-phenyl-1,3,8-triaza-spiro[4.5]dec-3-ylmethyl)-7H-pyrrolo[2,3-d]pyrimidine-2-carbonitrile trifluoroacetic acid salt (142 mg, 0.28 mol) in dichloromethane (2 ml), triethylamine (395 μl) and acetic anhydride (54 μl, 0.57 mmol) are added at 0° C. The reaction mixture is stirred for over night at room temperature, quenched with ice-water and extracted with ethyl acetate. The combined extracts are washed with H2O, brine and dried over sodium sulphate. Chromatography on silica gel gives 90 mg of 6-(8-acetyl-4-oxo-1-phenyl-1,3,8-triaza-spiro[4.5]dec-3-ylmethyl)-7-(2-cyclohexyl-ethyl)-7H-pyrrolo[2,3-d]pyrimidine-2-carbonitrile in 58% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07531546B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-9a8b9552e33a4d3faac084728bd36577 |
| Source note | uspto-grants-2009_05 |