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Acetic Acid → Styrenesulfonic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Aminobenzenesulfonic acid | HCID 6926 | — |
| 反応物 | Pentyl nitrite | HCID 10026 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 触媒 | (1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium | HCID 6505921 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Styrenesulfonic acid | HCID 168625 | 87.5% |
反応手順
13.0 g of aniline-2-sulphonic acid were suspended in 200 ml of methanol and treated with 20 g of glacial acetic acid. Under a nitrogen atmosphere, 9.5 g of amyl nitrite were added dropwise at a temperature of 0° to 5° C. and the suspension was stirred for 1 hour. A solution of 15 g of NaOH in 100 ml of methanol was then added dropwise at such a rate that the temperature of the mixture did not exceed 20° C. After addition of 0.5 g of bis(dibenzylideneacetone)palladium(0), the mixture was stirred at 20° C. for 3 hours under an ethylene pressure of 20 bar, the solid was then filtered off with suction and the filtrate was evaporated to dryness. 12.1 g (78%) of styrene-2-sulphonic acid, Na salt, were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05231223 |
| 出典データセット | uspto-grants-1993_07 |
| ORD ID | ord-48b29c1265524e6db3ea7f6337d420ad |
| 出典メモ | uspto-grants-1993_07 |