HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 178510458, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Hydroxybutanedinitrile | HCID 21253562 | — |
| Reactant | HCID 86607778 | HCID 86607778 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178510458 | HCID 178510458 | — |
Reaction Steps
6.1 g of malonitrile is dissolved in 100 mL of dimethylformamide. To the solution, in several portions, 3.6 g of 60% oily dispersion of sodium hydride are added. To the clear solution 18 g of 5-(4-benzylpiperazin-1-yl)isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The reaction mixture is diluted with 100 mL of water and extracted with 2×50 mL of ethyl acetate. The aqueous phase is evaporated in vacuum, the solid residue is dissolved in 50 mL of water, the pH is adjusted to 6 with acetic acid and refluxed for 5 hours. After cooling the precipitated material is filtered off, washed with water. After drying 14.3 g of the title compound is obtained, m.p.: 291° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07547696B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-29b029b0c4cf4e9aacb0593533032947 |
| Source note | uspto-grants-2009_06 |