HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dichloromethane → HCID 57378117, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| Edukt | 4-Amino-2-nitrobenzoic Acid | HCID 235713 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 57378117 | HCID 57378117 | 89% |
Reaktionsschritte
Triethylamine (55.8 μL, 0.4 mmol) and thiocarbonyldiimidazole (46.3 mg, 0.26 mmol) were added to a methylene chloride solution (0.4 mL) of 4-amino-2-nitrobenzoic acid (36.4 mg, 0.2 mmol) at room temperature, followed by stirring at room temperature for 10 minutes. The reaction mixture was dissolved in ethyl acetate and washed with 1 M hydrochloric acid, the organic layer was separated, and then the organic layer was dried over magnesium sulfate. Thereafter, filtration and concentration under reduced pressure to dryness were carried out to obtain 4-isothiocyanato-2-nitrobenzoic acid as a colorless solid (40 mg, yield: 89%, HPLC purity: 96.4%)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09102602B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-3ec28024c9bd4081b8104eea24de2c4b |
| Quellennotiz | uspto-grants-2015_08 |