HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86711940, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 178465664 | HCID 178465664 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Product | HCID 86711940 | HCID 86711940 | 100% |
Reaction Steps
A solution of N′-(1-iminoethyl)-4-(4-(trifluoromethoxy)phenyl)thiazole-2-carbohydrazide (10.0 g, 33.0 mmol) in ethylene glycol (20 mL) was stirred at 180° C. for 2 h. After cooling to RT, H2O (100 mL) was added and the mixture was extracted with EtOAc (2×100 mL). The combined organic layers were washed with brine (100 mL), dried over Na2SO4, filtered and concentrated under reduced pressure; the residue was purified by silica gel column chromatography (Petroleum ether:EtOAc=5:1) to afford the title compound as a white solid (9.6 g, 100%). MS (ES+) C13H9F3N4OS requires: 326. found: 327 [M+H]+; 1H NMR (500 MHz, DMSO) 8.27 (s, 1H), 8.15 (d, J=8.5 Hz, 2H), 7.48 (d, J=8.0 Hz, 2H), 2.43 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09018380B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-2fb116785f0e4dac8ce870e9740867e6 |
| Source note | uspto-grants-2015_04 |