HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl trifluoromethyl ketone → HCID 178465586, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl trifluoromethyl ketone | HCID 9871 | — |
| Reactant | 3-Chloro-2-hydrazinylpyridine | HCID 556100 | — |
| Reactant | HCID 178514363 | HCID 178514363 | — |
| Product | HCID 178465586 | HCID 178465586 | 66% |
Reaction Steps
1,1,1-Trifluoroacetone (7.80 g, 69.6 mmol) was added to 3-chloro-2(1H)-pyridinone hydrazone (alternatively named (3-chloro-pyridin-2-yl)-hydrazine) (10 g, 69.7 mmol) at 20-25° C. After the addition was complete, the mixture was stirred for about 10 minutes. The solvent was removed under reduced pressure and the mixture partitioned between ethyl acetate (100 mL) and saturated aqueous sodium carbonate solution (100 mL). The organic layer was dried and evaporated. Chromatography on silica gel (eluted with ethyl acetate) gave the product as an off-white solid (11 g, 66% yield), m.p. 64-64.5° C. (after crystallization from ethyl acetate/hexanes).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09113630B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-3b1f672becf947c7985b3260d3e727df |
| Source note | uspto-grants-2015_08 |