HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Chloroperbenzoic acid → HCID 58504127, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Anilino-2-(methylthio)-5-pyrimidinecarboxamide | HCID 295821 | — |
| Reactant | HCID 58504252 | HCID 58504252 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 58504127 | HCID 58504127 | 27.5% |
Reaction Steps
3-Chloroperoxybenzoic acid (195 mg) was added to a 0° C. suspension of the compound prepared in Example 93 (100 mg) in dichloromethane (4 mL). The reaction was stirred one hour at room temperature. Diisopropylethylamine (0.669 mL) and the compound prepared in Example 9 (198 mg) were added and the mixture was stirred at room temperature for 18 hours. The reaction was diluted with ethyl acetate and sequentially washed with a saturated sodium bicarbonate solution and brine. The organics were dried over magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (concentrated aqueous ammonia:methanol:ethyl acetate=0.1:0.9:25) to obtain the title compound (51 mg) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08809538B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-2b81f81d2e8242fe8832b0d95e813af3 |
| Source note | uspto-grants-2014_08 |