HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine hydrochloride → HCID 178427888, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine hydrochloride | HCID 11130 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 12045115 | HCID 12045115 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178427888 | HCID 178427888 | 50% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
[2,3-Difluoro-6-cyano-phenyl]-(4-iodo-2-methyl-phenyl)-amine (1.11 g, 3 mmol) and Sodium azide(0.255 g, 3.9 mmol) and triethylamine hydrochloride (0. 537 g, 3.9 mmol) were all suspended in 10 ml toluene and stirred at 100° C. for 12 hours. The mixture was concentrated and the residue purified by column chromatography with ethyl acetate/methanol (10/1) to give the product as a foam-like solid. The yield: ˜50% m.p: 83.4-88.7° C. 1H NMR(CDCl3, 400 Hz): δ/ppm 7.69(1H, m, Phenyl-H); 7.42(1H, s, Phenyl-H); 7.27(1H, m, Phenyl-H); 6.91(1H, dd, J=16.2 Hz, 8.3 Hz, Phenyl-H); 6.40(1H, dd, Phenyl-H); 2.28(3H, s, CH3)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06545030B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-e4346d745fd141588887a9e90494faac |
| Source note | uspto-grants-2003_04 |