HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 131727396, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 57634650 | HCID 57634650 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131727396 | HCID 131727396 | — |
Reaction Steps
To a cold (0° C.) solution of tert-butyl 4-{[2-(4-fluorobenzyl)-8,9-dihydroxy-1,6-dioxo-1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrazin-7-yl]methyl}piperidine-1-carboxylate (1.12 g, 2.23 mmol) in methylene chloride (10 mL), trifluoroacetic acid (3.4 mL, 45 mmol) was added and the mixture was stirred for 2 hours. The mixture was concentrated in vacuo and the residue was purified by prep HPLC (Waters prep LC 4000 System using a Waters Nova Pak column [3*10×40 mm I.D. cartridges, C18, 6 μM pore size) eluting with 95-5% water (0.10% TFA)/acetonitrile (0.10% TFA) gradient at 60 mL/min]. Combined and concentrated the product fractions to give a yellow solid. The solids were triturated with acetonitrile and collected by vacuum filtration.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07517532B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-f38777628fb745c6bc36ebe88dbc492e |
| Source note | uspto-grants-2009_04 |