HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 9799262, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,2-Dimethylpropylamine | HCID 11731 | — |
| Reactant | HCID 178512266 | HCID 178512266 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 9799262 | HCID 9799262 | 59% |
Reaction Steps
A solution of N-[3,5-bis(trifluoromethyl)phenyl]-N'-cyano-O-phenylisourea (0.8 mmol, 300 mg), 3-methyl-2-butylamine (0.88 mmol, 0.101 ml) and triethylamine (0.88 mmol, 0.123 ml) in acetonitrile (2 ml) was stirred for 7 h at 75° C. After concentration the residue was dissolved in ethyl acetate, washed with water, dried (Na2SO4) and concentrated. The residue was purified by column chromatography (heptane:ethyl acetate 4:1) to give the title compound (143 mg, 59%) as white crystals. Mp 134-136° C.; EI SP/MS: 366 (M+); 1H-NMR (CDCl3): δ 0.92 (d, 6H),1.15 (d, 3H), 1.78 (m, 1H), 3.78 (m, 1H), 4.85 (br, 1H), 7.73 (br s, 3H), 8.0 ppm (br, 1H); MA calc for C15H16F6N4 :C, 49.18%; H, 4.40%; N, 15.29%. Found: C, 48.95%; H, 4.38%; N 15.08%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06147098 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-dbb96d4c33434c778e70dd328edecd85 |
| Source note | uspto-grants-2000_11 |