HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 22901847, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 22901841 | HCID 22901841 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 22901847 | HCID 22901847 | — |
Reaction Steps
75 ml of aqueous methylamine solution (40%) are added to a solution of 12.6 g of 2,3-dihydro-2-oxo-3-tert-butylcarbonylmethyl-5-trifluoromethyl-1,3,4-oxadiazole in 50 ml of acetonitrile. After the slightly exothermal reaction has subsided, the reaction mixture is stirred for 2 hours at room temperature and then for 14 hours at 80° and then evaporated the liquid residue is treated with ice-water, and the aqueous mixture is extracted three times by shaking with ethyl acetate. The combined ethyl acetate phases are dried and evaporated, and the oily orange residue is recrystallized from hexane. This gives the title compound in the form of pale yellow crystals which melt at 100°-105°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05679623 |
| Source dataset | uspto-grants-1997_10 |
| ORD ID | ord-8bb9ce9ce7d341509fa44d8a1073ac34 |
| Source note | uspto-grants-1997_10 |