HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 58266511, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 58266327 | HCID 58266327 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58266511 | HCID 58266511 | 78.4% |
Reaction Steps
Trifluoroacetic acid (30 mL) was added to a solution of (5-bromo-6-chloro-4-iodo-pyridin-3-yl)-carbamic acid tert-butyl ester (19.0 g, 44 mmol) in DCM (120 mL) and the resultant solution was stirred at ambient temperature for 2 h then concentrated in vacuo. The resultant residue was loaded onto an SCX-2 cartridge (70 g) eluting with acetonitrile (100 mL) then 2N ammonia in methanol (100 mL). The basic fraction was concentrated in vacuo to afford the title compound (11.5 g, 78%). 1H NMR (DMSO-D6, 400 MHz): 7.23 (s, 1H), 5.92 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09216980B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-f4be0d483a4549f59a9fe19e2a5dbf39 |
| Source note | uspto-grants-2015_12 |