HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 54112244, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Chlorobenzene | HCID 7964 | — |
| Reactant | 3-Oxabicyclo(3.1.0)hexane-2,4-dione | HCID 2734721 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 54112244 | HCID 54112244 | — |
Reaction Steps
4.5 g (0.040 mol) of chlorobenzene and 5.0 g (0.0446 mol) of 1,2-cyclopropanedicarboxylic acid anhydride were successively added dropwise to a mixture of 60.0 g (0.45 mol) of anhydrous aluminium chloride and 9 mL (0.115 mol) of anhydrous dimethylformamide while maintaining a reaction temperature of 60° C. to 70° C. and the mixture was then kept at 70° C. for 1 hour. After cooling, the reaction mixture was stirred into a mixture of 500 g of crushed ice and 60 mL of concentrated hydrochloric acid, the precipitate was suction filtered, washed thoroughly with water and dried over Siccapent in a vacuum drying chamber at a temperature of 50° C. 7.8 g (87% of theoretical) of colorless crystals were obtained, m.p. 150° C.-153° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07407963B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-7ab29fdcda124147be1fe219a48166a4 |
| Source note | uspto-grants-2008_08 |