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2-Pyridinyl-1,3-dioxolane → 1-(2,5-Dibromobenzyl)-2-(1,3-dioxolan-2-yl)pyridinium bromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Pyridinyl-1,3-dioxolane | HCID 79773 | — |
| 反応物 | 1,4-Dibromo-2-(bromomethyl)benzene | HCID 5326038 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Sulfolane | HCID 31347 | — |
| 生成物 | 1-(2,5-Dibromobenzyl)-2-(1,3-dioxolan-2-yl)pyridinium bromide | HCID 19047503 | 157.2% |
反応手順
A mixture of 25.03 g (0.165 mol) of 2-(1,3-dioxolan-2-yl)pyridine and 2,5-dibromobenzyl bromide (54 g, 0.165 mol) in 60 mL of sulfolane was heated on a steam-bath for 6 h. The mixture was diluted with 600 mL of ethyl acetate, cooled, and the resulting solid product was isolated by filtration. The above solid was triturated in 300 mL of ethyl acetate, the mixture was cooled, filtered and dried to afford 62.24 g (79%) of 1-(2,5-dibromobenzyl)-2-(1,3-dioxolan-2-yl)pyridinium bromide (Formula VI: R1 =R2 =H; R7 =2,5-Br2 ; Z- =Br-), as a yellow solid, m.p. 135°-139° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05554620 |
| 出典データセット | uspto-grants-1996_09 |
| ORD ID | ord-765e1ed5c3214074bbde20da683aad41 |
| 出典メモ | uspto-grants-1996_09 |