HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenolate Sodium → HCID 67064578, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenolate Sodium | HCID 4445035 | — |
| Reactant | N-(7-chloro-2-methylpyrazolo[1,5-a]pyrimidin-5-yl)-4-(2-hydroxypropan-2-yl)benzamide | HCID 86652267 | — |
| Catalyst | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 67064578 | HCID 67064578 | 37.5% |
Reaction Steps
A solution of N-(7-chloropyrazolo[1,5-a]pyrimidin-5-yl)-4-(2-hydroxypropan-2-yl)benzamide (2D, 100 mg, 0.302 mmol) and sodium phenoxide (70 mg, 605 mmol) in NMP (3 mL) was stirred at room temperature overnight. After cooling to room temperature, the mixture was diluted with a few drops of DMSO and methanol, and was then purified by preparatory HPLC, 40-50% (MeCN/H2O gradient+0.01% TFA). Lyophilization of the combined fractions gave the titled compound as a white solid (44 mg, 37%). 1H NMR (DMSO-d6) δ: 11.11 (s, 1H), 8.21 (d, J=2.3 Hz, 1H), 7.91 (d, J=8.6 Hz, 2H), 7.41-7.68 (m, 7H), 7.17 (s, 1H), 6.51 (d, J=2.3 Hz, 1H), 3.94 (br. s., 1H), 1.43 (s, 6H). ESI-MS: m/z 389.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461163B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-3806d7dbd7564e4b8d125837d0945d6a |
| Source note | uspto-grants-2013_06 |