HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 58586423, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Bromo-1,1,1-trifluorobutane | HCID 521006 | — |
| Reactant | tert-Butyl 3,3-dicyanopropanoate | HCID 58586409 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58586423 | HCID 58586423 | 67.9% |
Reaction Steps
0.48 g of 2-(tert-butoxycarbonylmethyl)malononitrile and 0.32 g of 1,1,1-trifluoro-4-bromobutane were dissolved in 2 ml of N,N-dimethylformamide, and to the solution was added 0.40 g of potassium carbonate followed by stirring for 5 hours at room temperature. Then, to the reaction mixture was added dilute hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was subjected to silica gel column chromatography to give 0.33 g of 2-(tert-butoxycarbonylmethyl)-2-(4,4,4-trifluorobutyl)malononitrile (hereinafter referred to as the present invention compound (51)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07439266B2 |
| Source dataset | uspto-grants-2008_10 |
| ORD ID | ord-d35b10c84cd14ef4837d69d9c895df03 |
| Source note | uspto-grants-2008_10 |