Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | 2-Chlorobenzene-1-carboperoxoic acid | HCID 12587398 | — |
| Reactant | HCID 86732468 | HCID 86732468 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 71554404 | HCID 71554404 | — |
Reaction Steps
To a solution of 1.24 g 2-[1-(4-ethoxy-2,6-difluorobenzyl)-1H-indazol-3-yl]-5-[2-(methylsulfanyl)ethoxy]-N-(pyridin-4-yl)pyrimidin-4-amine (4-16, 2.26 mmol, 1. eq.) in 2.15 ml of dry chloroform, was added slowly at 0° C. a solution of 557 mg 2-chlorobenzenecarboperoxoic acid (77%, 2.49 mmol, 1.1 eq.) in 2.15 ml chloroform. After 30 min dichloromethane and sodium thiosulfate-solution (10%) were added. The slurry was stirred for 5 min. After separating the solid (product) the aqueous layer was washed with dichloromethane twice. The organic layers were dried with sodium sulphate and concentrated in vacuo. The residue was purified by flash chromatography and combined the former isolated solid to yield 1.22 g (2.05 mmol, 91%) of the analytically pure target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09265763B2 |
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| Source dataset | uspto-grants-2016_02 |
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| ORD ID | ord-d065e187502845d7b5999bc5fbe77b52 |
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| Source note | uspto-grants-2016_02 |
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