HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22249670, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Butyryl chloride | HCID 8855 | — |
| Reactant | HCID 135593034 | HCID 135593034 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22249670 | HCID 22249670 | 42.4% |
Reaction Steps
Triethylamine (0.091 mL, 0.652 mmol) was added to a solution of 3-mesityl-2,5-dimesityl-7,8-dihydro-6H-pyrazolo[1,5-a]pyrrolo[3,2-e]pyrimidine (100 mg, 0.326 mmol) which was prepared in Example 71 in dichloromethane (4 mL), butyryl chloride (0.037 mL, 0.358 mmol) was added dropwise at room temperature, followed by stirring for two hours. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate, washed with brine, and then dried over MgSO4. The solvent was evaporated, and the residue was subjected to silica gel column chromatography (7 g), to give the title compound (52 mg, 42%) as a pale yellow oil from a fraction of ethyl acetate-hexane (1:4 v/v).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06927221B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-d3695d448b9c40feb468d76b188ba855 |
| Source note | uspto-grants-2005_08 |