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1,2-Dihydro-6-methyl-2-oxo-5-phenyl-3-pyridinecarbonitrile → 2-Chloro-6-methyl-5-phenylnicotinonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dihydro-6-methyl-2-oxo-5-phenyl-3-pyridinecarbonitrile | HCID 20231 | — |
| 反応物 | Phenylphosphonic dichloride | HCID 69990 | — |
| 生成物 | 2-Chloro-6-methyl-5-phenylnicotinonitrile | HCID 1476365 | 85% |
反応手順
A mixture of 100.34 g 3-cyano-6-methyl-5-phenyl-1H-pyridin-2-one [Walker and Weaver, J. Org. Chem. 26, 4441 (1961)] and 192 ml phenylphosphonic dichloride (C6H5POCl2) was warmed to 160°-170° C. and kept at that temperature for about 16 hours. The reaction mixture was cooled and poured into ice water. The solid product was collected, dried in a vacuum oven and extracted with ether. The ether solution was concentrated, and the residue was washed with hexane and extracted with 300 ml 15% aqueous potassium bicarbonate. The resulting solid was dried in a vacuum oven to give 92.71 g (85%) 2-chloro-3-cyano-6-methyl-5-phenylpyridine, m.p. 134°-135° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05010086 |
| 出典データセット | uspto-grants-1991_04 |
| ORD ID | ord-778b9871528946f18e36b335d199c984 |
| 出典メモ | uspto-grants-1991_04 |