HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 11391634, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1-Octanethiol | HCID 8144 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,2-Benzenedicarbonitrile, 4-nitro- | HCID 97443 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 11391634 | HCID 11391634 | 68% |
Reaction Steps
While cooling a reaction vessel on a water bath, were mixed 17.3 g (100 mmol) of 4-nitrophthalonitrile, 15.7 g (110 mmol) of 1-octanethiol, 20.7 g (150 mmol) of potassium carbonate and 80 ml of N,N-dimethylacetamide. The resultant mixture was stirred for 7 hours at room temperature and then for 1 hour at 40° C. The thus-obtained reaction mixture was poured into 600 ml of a 3% hydrochloric acid. The resultant precipitates were separated by a filtration under reduced pressure, and then washed with water and dried. Thereafter, by recrystallization from a mixed solvent of methanol (190 ml)/water (9 ml), there was obtained 18.5 g (Yield: 68%) of white powder synthesis intermediate (A-1) (Melting point=37 to 38° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07947826B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-6bbefa36595a4352bf94931a18fe2a0f |
| Source note | uspto-grants-2011_05 |