HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 86695063, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178499492 | HCID 178499492 | — |
| Product | HCID 86695063 | HCID 86695063 | 84% |
Reaction Steps
To methyl 2-(2-(3-(benzyloxy)phenyl)-7-hydroxy-5-methylpyrazolo[1,5-a]pyrimidin-6-yl)acetate (0.3 g, 0.75 mmol) was added POCl3 (3 mL). The reaction mixture was heated at reflux for 2 h. After cooling, the reaction mixture was added drop-wise to ice-water. A brown solid precipitated. The solid was filtered and washed with water, then dissolved in ethyl acetate. The organic solution was washed with saturated NaHCO3 and dried over sodium sulfate. The solvent was evaporated to give the title compound (2.77 g, 84%). 1H-NMR (400 MHz, DMSO-d6) δ 2.56 (s, 3H), 3.69 (s, 3H), 4.01 (s, 2H), 5.20 (s, 2H), 7.10 (dd, 1H), 7.29 (s, 1H), 7.32-7.37 (m, 1H), 7.39-7.45 (m, 3H), 7.51 (d, 2H), 7.63-7.69 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034882B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-44321958687a4d6eb6471d4fe39ec9fc |
| Source note | uspto-grants-2015_05 |