HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 59285281, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 67135219 | HCID 67135219 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59285281 | HCID 59285281 | 30.8% |
Reaction Steps
Trifluoroacetic Acid (1 mL) was added to a solution of tert-butyl 4-({2-(3-{[tert-butyl(dimethyl)silyl]oxy}-2,2-dimethylpropyl)-6-[5-(cyclopropylcarbamoyl)-3-fluoro-2-methylphenyl]-1-oxo-1,2-dihydroisoquinolin-4-yl}sulfonyl)piperidine-1-carboxylate (Example 60a, 0.116 g) in DCM (2 mL), and the reaction was stirred at room temperature for 30 min. The reaction was then azeotroped with toluene (3×10 mL), and the residue dissolved in methanol and purified by preparative HPLC (Phenomenex Gemini column using a 95-5% gradient of 0.2% aqueous NH3 in MeCN). Solvent removal and trituration with diethyl ether gave the title compound (0.026 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08012980B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-b6cab498ddc1466ca9117e076344339a |
| Source note | uspto-grants-2011_09 |