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Methyl trifluoromethyl ketone → HCID 178465586、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl trifluoromethyl ketone | HCID 9871 | — |
| 反応物 | 3-Chloro-2-hydrazinylpyridine | HCID 556100 | — |
| 反応物 | HCID 178514363 | HCID 178514363 | — |
| 生成物 | HCID 178465586 | HCID 178465586 | 66% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179824B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-7069031da38e4f3b9580938ff670e6e7 |
| 出典メモ | uspto-grants-2007_02 |