関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Formate | HCID 2723810 | — |
| 反応物 | 4-Chloro-3-methylbut-2-en-1-yl acetate | HCID 53400932 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Acetoxy-2-methyl-2-buten-1-ol formate | HCID 54335244 | 95% |
反応手順
4-Acetoxy-2-methyl-1-chloro-2-butene (8.13 g, 50 mmol) was dissolved in dimethylformamide (25 ml) and placed in a 100 ml four neck flask. To this were added sodium formate powder (6.80 g, 100 mmol, 2 equivalents) and tetra n-butylammonium bromide (0.81 g, 2.5mmol, 5 mol %). The mixture was stirred at 40° C. for 24 hours under heating. After completion of the reaction, the reaction mixture was poured into ice-cooled water (about 30 ml)and extracted with ether (50 ml) three times. The extracted ether layer was dried over anhydrous sodium sulfate. Evaporation of the ether followed by purification by silica gel column chromatography (ethyl acetate-hexane (=1:3)) gave 4-acetoxy-2-methyl-2-buten-1-ol formate (8.18 g, 47.5 mmol; Yield: 95.0%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424478 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-af0afce5ae2b4b0883b9351102509ab8 |
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| 出典メモ | uspto-grants-1995_06 |
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