HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 72202968, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 123859023 | HCID 123859023 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 72202968 | HCID 72202968 | — |
Reaction Steps
32.7 mg of 4-({5-(2-{[tert-butyl(dimethyl)silyl]oxy}ethoxy)-2-[1-(2-fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazol-3-yl]pyrimidin-4-yl}amino)nicotinonitrile 2-3-10 (0.034 mmol, 1.00 eq.) were dissolved in 0.58 mL dioxane and 0.085 mL 4 M hydrochloric acid in dioxane (0.341 mmol, 10.0 eq.) were added and stirred at rt over night. The reaction mixture was partitioned between half saturated aqueous ammonium chloride solution and DCM/isopropanol (4:1). The combined organic layers were washed with brine, dried over silicon filter and concentrated in vacuo. The residue was purified by preparative thin layer chromatography (DCM/methanol (9:1)) to provide 8.7 mg (0.02 mmol, 54%) of analytically pure target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09416125B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-eaf74374fd63472db3277420fdd65327 |
| Source note | uspto-grants-2016_08 |