HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thionyl Chloride → HCID 14279665, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 14347810 | HCID 14347810 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 14279665 | HCID 14279665 | 78.8% |
Reaction Steps
N,N-dimethylformamide (3 drops) was added to a mixture consisting of 2-[4-carbamoylmethyl-7-fluoro-2H-1,4-benzoxazin-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (0.2 g), toluene (30 ml) and thionyl chloride (0.2 g), and then the mixture was refluxed under heating for 3 hours. After the solvent was concentrated, toluene (50 ml) was added and fully mixed therewith, and then toluene was distilled off. The resulting solid was recrystalled from ethanol to give the desired 2-[4-cyanomethyl-7-fluoro-2H-1,4-benzoxazin-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (0.15 g). mp. 225°-229° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04798620 |
| Source dataset | uspto-grants-1989_01 |
| ORD ID | ord-6facb16927f34d51be7e96de3080bb5f |
| Source note | uspto-grants-1989_01 |