HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylhydrazine → Ethyl 3-difluoromethyl-1-methyl-4-pyrazole carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylhydrazine | HCID 6061 | — |
| Reactant | [(E)-3-(dimethylamino)-2-ethoxycarbonyl-4,4-difluorobut-2-enylidene]-dimethylazanium tetrafluoroborate | HCID 178472002 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Ethyl 3-difluoromethyl-1-methyl-4-pyrazole carboxylate | HCID 11644126 | — |
Reaction Steps
10.0 g (30 mmol) of N-[(2E)-1-(difluoromethyl)-3-(dimethylamino)-2-(ethoxycarbonyl)prop-2-en-1-ylidene]-N-methylmethanaminium tetrafluoroborate were dissolved in 50 ml of acetonitrile and admixed with 2.3 g of methylhydrazine. After stirring at RT for 2 h, the acetonitrile was removed completely under reduced pressure. Distillation under reduced pressure or crystallization from n-hexane afforded 5.3 g (86% of theory) of the product having an m.p. of 63-65° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07939673B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-7fdf5d01d81a4c53b28ce68e38b82729 |
| Source note | uspto-grants-2011_05 |