HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 22340996, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Thiophosgene | HCID 10040 | — |
| Reactant | 4-chloro-2-fluoro-5-(2-pyrimidinyloxy)aniline | HCID 11447802 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22340996 | HCID 22340996 | — |
Reaction Steps
4-Chloro-2-fluoro-5-(2-pyrimidinyloxy)-benzenamine (50 g) and triethyl amine (42.2 g) were dissolved in anhydrous ethyl acetate (400 ml) and stirred under ice cooling. Thiophosgene (74.3 g) dissolved in ethyl acetate (400 ml) was slowly added to the stirred solution. The mixture was heated at reflux for 2 hr and filtered. Evaporation of the solvent afforded 2-(2-chloro-4-fluoro-5-isothiocyanatophenoxy)-pyrimidine which was used for the next step without purification. 1H NMR, CDCl3, 7.12 (1H, t, J=4.7 Hz), 7.13 (1H, d, J=7.0 Hz), 7.32 (1H, d, J=8.9 Hz), 8.58 (2H, t, J=4.7 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06613718B2 |
| Source dataset | uspto-grants-2003_09 |
| ORD ID | ord-f8787ca8e2f74f6e93fa2ec77724f03b |
| Source note | uspto-grants-2003_09 |