HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → Methyl 2-tert-butoxy-2-(3,7-dichloro-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-yl)acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Perchloric Acid | HCID 24247 | — |
| Reactant | Methyl 2-(3,7-dichloro-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-yl)-2-hydroxyacetate | HCID 86670282 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | tert-Butyl acetate | HCID 10908 | — |
| Product | Methyl 2-tert-butoxy-2-(3,7-dichloro-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-yl)acetate | HCID 86670283 | 181.5% |
Reaction Steps
To a suspension of methyl 2-(3,7-dichloro-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-yl)-2-hydroxyacetate (80 mg, 0.26 mmol) in tert-butyl acetate (1.5 mL) at room temperature was added CH2Cl2 (1.5 mL) followed by perchloric acid (40 mg, 2.1 mmol). The reaction mixture was stirred for 2 h at room temperature. The reaction mixture was diluted with ethyl acetate (15 mL). The organic phase was washed with saturated NaHCO3 (2×10 mL), followed by water (1×10 mL) and dried over sodium sulfate. The solvent was evaporated. Purification by silica gel chromatography provided the title compound (85 mg, 90%). Used as is in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08633200B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-8ef0189e279e4c98b063051719800651 |
| Source note | uspto-grants-2014_01 |