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Acetic Anhydride → 1-Phenyl-2-acetoxy-cyclohex-3-ene-1-carboxylic acid-ethyl-ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl 2-phenylacrylate | HCID 89651 | — |
| 反応物 | Crotonaldehyde | HCID 447466 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 生成物 | 1-Phenyl-2-acetoxy-cyclohex-3-ene-1-carboxylic acid-ethyl-ester | HCID 21394564 | — |
反応手順
1 mole (170 g) of ethyl atropate, 210 g of crotonaldehyde, 150 g of anhydrous sodium acetate and 0.6 of acetanhydride are heated to boiling for 6 h. while stirring. Subsequently the main amount of the liquid phase is distilled off under vacuum, and the residue is extracted with 1 liter of hot ligroin. The residue of the ligroin phase is distilled. The product -- although being pure according to gas chromatography -- distills in a wide boiling range: b.p. °, 1 130°-165° C. Yield: 105 g. It crystallizes when allowed to stand. M.P. 72°-73° C (from petroleum ether).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04061635 |
| 出典データセット | uspto-grants-1977_12 |
| ORD ID | ord-01f0f2e335a4496fa45d9785f3606c18 |
| 出典メモ | uspto-grants-1977_12 |