HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 9881898, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Reactant | 2-Cyanoethanethioamide | HCID 1416277 | — |
| Reactant | HCID 12715559 | HCID 12715559 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 9881898 | HCID 9881898 | — |
Reaction Steps
2-Propoxyacetophenone (2.14 g) and dimethylformamide dimethylacetal (2 ml) were heated together in dimethyl-formamide (10 ml) at 130° C. for 18 hours. Cyanothioacetamide (1.6 g) was added, heating was continued for 2 hours, and the cool mixture was poured into water (100 ml). The aqueous mixture was neutralized with acetic acid and extracted with ethyl acetate. Evaporation of the extract gave a residue which was purified by medium pressure chromatography (silica, dichloromethane:methanol mixtures) to give a solid, 0.35 g, m.p. 127°-128° C. Recrystallization from aqueous ethanol afforded the pure title compound, 0.22 g, m.p. 130°-131° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06046216 |
| Source dataset | uspto-grants-2000_04 |
| ORD ID | ord-06856e4b4f9442b4a0e0c661338dd7fa |
| Source note | uspto-grants-2000_04 |