HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1-Dimethylhydrazine → HCID 70654257, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1-Dimethylhydrazine | HCID 5976 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Chloropyridine-2-carbonyl chloride--hydrogen chloride (1/1) | HCID 22397270 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 70654257 | HCID 70654257 | 56% |
Reaction Steps
To a suspension of 4-chloropicolinoyl chloride hydrochloride (352 mg, 2.0 mmol, 1.0 eq) in 10 mL of THF were added N,N-dimethylhydrazine (120 mg, 2.0 mmol, 1.0 eq) and N,N-diisopropylethylamine (383 μL, 2.2 mmol, 1.1 eq) at room temperature. The reaction mixture was stirred for 15 min and diluted with water (25 mL) and EtOAc (50 mL). The separated organic layer was washed with brine (25 mL), saturated sodium bicarbonate solution (25 mL) and dried over sodium sulfate. Concentration under reduced pressure gave the title compound as colorless solid (223 mg, 56%), which was used without further purification. MH+=200, Rt=1.42 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08710048B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-c9d58abdaf3f4611b162f78c9c57e502 |
| Source note | uspto-grants-2014_04 |