関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloride | HCID 312 | — |
| 反応物 | 1-Bromo-2-Chloroethane | HCID 7849 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzyltriethylammonium | HCID 17208 | — |
| 反応物 | 2,2-Difluoro-1,3-benzodioxole-5-acetonitrile | HCID 20311384 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2,2-Difluorobenzo[D][1,3]dioxol-5-YL)cyclopropanecarbonitrile | HCID 57446150 | — |
反応手順
Sodium hydroxide (50% aqueous solution, 10 mL) was slowly added to a mixture of crude (2,2-difluoro-benzo[1,3]dioxol-5-yl-acetonitrile, benzyltriethylammonium, chloride (3.00 g, 15.3 mmol), and 1-bromo-2-chloroethane (4.9 g, 38 mmol) at 70° C. The mixture was stirred overnight at 70° C. before the reaction mixture was diluted with water (30 mL) and extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and evaporated to dryness to give crude 1-(2,2-difluoro-benzo[1,3]dioxol-5-yl)-cyclopropanecarbonitrile, which was used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524910B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-b5f7da59d0044b58b7f926938dd088e6 |
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| 出典メモ | uspto-grants-2013_09 |
|---|
