HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → (3,5-Dihydroxypicolinoyl)glycine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | [(3,5-Dihydroxy-pyridine-2-carbonyl)-amino]-acetic acid tert-butyl ester | HCID 59513079 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (3,5-Dihydroxypicolinoyl)glycine | HCID 24891198 | 89% |
Reaction Steps
To a solution of [(3,5-dihydroxy-pyridine-2-carbonyl)-amino]-acetic acid tert-butyl ester, 28, (0.10 g, 0.37 mmol) in CH2Cl2 (4 mL) at room temperature is added trifluoroacetic acid (1 mL). The reaction is stirred for 16 hours at room temperature and then concentrated under reduced pressure. The solid that remains is collected by filtration, washed with Et2O to afford 0.070 g (89% yield) of the desired compound as a colorless solid. 1H NMR (250 MHz, DMSO-d6) δ ppm 10.86 (1H, br s), 9.00 (1H, t, J=6.1 Hz), 7.77 (1H, d, J=2.4 Hz), 6.69 (1H, d, J=2.4 Hz), 3.95 (1H, d, J=6.2 Hz). HPLC-MS: m/z 213 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598210B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-830497372df64f14b72d8555b7717d2f |
| Source note | uspto-grants-2013_12 |