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4-Methylbenzaldehyde → 2-(2-p-Tolyl-vinyl)-pyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylbenzaldehyde | HCID 7725 | — |
| 反応物 | 2-Methylpyridine 1-oxide | HCID 13602 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(2-p-Tolyl-vinyl)-pyridine 1-oxide | HCID 69592129 | 55% |
反応手順
To a refluxing solution of 2-picoline-1-oxide (10.9 g, 100 mmol), potassium tert.-butanolate ( 11.2 g, 100 mmol) in butanol (100 ml) was added portion-wise p-tolualdehyde (12.0 g, 100 mmol). Reflux was maintained for 90 min. Then the mixture was cooled to rt, diluted with H2O (100 ml) and extracted with CH2Cl2. The combined organic phases were dried with MgSO4, concentrated and chromatographed (SiO2 with CH2Cl2/MeOH=95:5) to provide the title compound (11.6 g, 55%) as a yellow solid material. MS: m/e=211 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06951875B2 |
| 出典データセット | uspto-grants-2005_10 |
| ORD ID | ord-a495954aa2bd448ba35baf9716c9dcc7 |
| 出典メモ | uspto-grants-2005_10 |