HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178507517, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 2-(2-Aminophenyl)sulfanylbenzonitrile | HCID 366233 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178507517 | HCID 178507517 | 66.5% |
Reaction Steps
In 25 ml of DMF were suspended 2.4 g of 2-(2-aminophenylthio)benzonitrile (prepared in accordance with Reference Example 5, Step 4), 3.4 g of sodium azide and 1.7 g of ammonium chloride and the suspension was stirred at 110°-120° C. for 5 hours. After cooling, the reaction mixture was diluted with water, acidified with acetic acid and extracted with ethyl acetate. The extract was washed with water, dried and concentrated and the residue was crystallized from ethyl acetate and isopropyl ether to give 1.9 g of the title compound as white crystals, m.p. 153°-156° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05399703 |
| Source dataset | uspto-grants-1995_03 |
| ORD ID | ord-43ac6c55903d4dd3a5b6d0b01679396f |
| Source note | uspto-grants-1995_03 |