HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 178505621, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 59177869 | HCID 59177869 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 178505621 | HCID 178505621 | — |
Reaction Steps
A solution of 2.00 g (8.01 mmol) of 1-(2-chloropyridin-3-yl)-2-(2-fluorophenyl)ethanone from example 11A and 560 mg (11.2 mmol) of hydrazine hydrate in 6 ml of 1-butanol is heated in a microwave at 200° C. for 10 min. It is then diluted with tert-butyl methyl ether, washed with saturated sodium bicarbonate solution and dried over sodium sulfate. The solution is concentrated in vacuo. The crystalline residue is stirred with a little tert-butyl methyl ether and filtered off with suction. The mother liquor is concentrated and purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 2:1). In total, 1.40 g (77% of theory) of the desired product are obtained as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309551B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-92fbb16f0f0f491cb71514a71c63f453 |
| Source note | uspto-grants-2012_11 |