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2,6-Dichloropyridine → 2-Chloro-6-(2-Thienylmethoxy)Pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Dichloropyridine | HCID 16989 | — |
| 反応物 | 2-Thiophenemethanol | HCID 69467 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 2-Chloro-6-(2-Thienylmethoxy)Pyridine | HCID 18186944 | 93% |
反応手順
K-t-BuO (1.70 g, 15.1 mmol) was added portionwise to a stirred mixture of 2-thiophenemethanol (2.14 g, 18.7 mmol) and 2,6-dichloropyridine (2.13 g, 14.4 mmol) in dioxane (3 mL) at room temperature. An exotermic reaction started and more dioxane (3 mL) was added. After 3 h of stirring at room temperature, the reaction mixture was passed through a column of silica using n-hexane/ethyl acetate (85:15) as eluent. A second purification on silica (16×4 cm) using n-hexane/ethyl acetate (9:1) furnished 3.0 g (93%) of the title compound as a light beige oil. HRMS m/z calcd for C10H8ClNOS (M)+ 225.0015, found 225.0022. Anal. (C10H8ClNOS) C, H, N.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06593330B2 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-2663316dfb26462a96dee5ad5313b43f |
| 出典メモ | uspto-grants-2003_07 |