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Cornforth reagent → (5-Chloro-2-nitro-phenyl)-(6-chloro-pyridin-3-yl)-methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cornforth reagent | HCID 2724130 | — |
| 反応物 | (5-Chloro-2-nitro-phenyl)-(6-chloro-pyridin-3-yl)-methanol | HCID 22327314 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (5-Chloro-2-nitro-phenyl)-(6-chloro-pyridin-3-yl)-methanone | HCID 22327306 | — |
反応手順
To (5-Chloro-2-nitro-phenyl)-(6-chloro-pyridin-3-yl)-methanol was added an excess (ca. 2 eq.) of PDC in DCM. The suspension was shaken at room temperature overnight. The reaction was monitored by LC-MS, another 1-2 eq. of PDC was added and the reaction was shaken for another 6 hours. The crude product was filtered through Celite and purified by flash chromatography (silica gel, DCM). 1H NMR (CDCl3): δ (ppm): 7.50 (d, J=2.4 Hz, 1H), 7.79 (d, J=8.0 Hz, 1H), 7.68 & 7.70 (dd, J=8.8 Hz, 2.0 Hz, 1H), 8.09-8.11 (m, 1 H), 8.24 (d, J=8.8 Hz, 1 H), 8.57 (d, J=2.0 Hz, 1 H. MS: (M+H)/z=296.9
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07420055B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-65646e9902364857ae21534a90002e81 |
| 出典メモ | uspto-grants-2008_09 |