HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 7-(2-{1-[4-Hydroxy-1-methyl-5-(4-trifluoromethylphenyl)-1H-pyrazol-3-yl]ethylidene}hydrazinecarbothioamido)-4H-benzo[1,4]oxazin-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| Edukt | 7-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 2764182 | — |
| Edukt | HCID 72360113 | HCID 72360113 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 7-(2-{1-[4-Hydroxy-1-methyl-5-(4-trifluoromethylphenyl)-1H-pyrazol-3-yl]ethylidene}hydrazinecarbothioamido)-4H-benzo[1,4]oxazin-3-one | HCID 76597763 | 49% |
Reaktionsschritte
7-Amino-4H-benzo[1,4]oxazin-3-one (33 mg, 0.203 mmol) was stirred with a dimethylformamide solution of thiocarbonyldiimidazole (0.1 M, 2.03 mL, 0.203 mmol) at room temperature for 1 hour and then with a dimethylformamide solution of 3-(1-hydrazonoethyl)-1-methyl-5-[4-(trifluoromethyl)phenyl]-1H-pyrazol-4-ol prepared in Reference Synthetic Example 14 (0.1 M, 1.36 mL, 0.135 mmol) at room temperature for 4 hours Water was added, and the precipitated solid was collected by filtration, washed with water and dried. After addition of chloroform, the solid was collected by filtration washed with chloroform and dried to give 33.6 mg of the desired product (yield 49%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08134013B2 |
| Quelldatensatz | uspto-grants-2012_03 |
| ORD ID | ord-c77f0600e5e24a03bf3250106be82b89 |
| Quellennotiz | uspto-grants-2012_03 |