HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 54454020, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 53828432 | HCID 53828432 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 54454020 | HCID 54454020 | — |
Reaction Steps
10 g of H2SO4 (98%) is added dropwise at 0°-5° C., in the course of 10 minutes, to a solution of 12.3 g of 1-ethylcyclopropanecarboxylic acid cyanide in 13 g of tert-butanol and 13 ml of methylene chloride. The solution is subsequently stirred for 4 hours at room temperature; 2 ml of H2O is then added and stirring is continued for a further 30 minutes. The pH value of the solution is brought to 6 with 80 ml of ZnNaOH, and the organic phase is separated. After removal of the solvent, the residue is crysrallised out from 50 ml of petroleum ether (b.p. 40° to 65° C.) at 50° C. to thus yield 13.1 g of white crystals of pure (1-ethylcyclopropyl)-glyoxylic acid tert-butylamide having a melting point of 37.5°-39° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04402733 |
| Source dataset | uspto-grants-1983_09 |
| ORD ID | ord-71904e831c64453ea4362c8dd92031d4 |
| Source note | uspto-grants-1983_09 |