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Iodine → (2-Ethyl-4-sulfanylphenoxy)acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphine | HCID 24404 | — |
| 反応物 | Ethyl 2-(4-(chlorosulfonyl)-2-ethylphenoxy)acetate | HCID 21986343 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | (2-Ethyl-4-sulfanylphenoxy)acetic acid | HCID 17951787 | — |
反応手順
To a refluxing solution of PH3 (4.3 g, 126.5 mmol) and I2 (0.7 g, 2.6 mmol) in glacial acetic acid (30 ml) was added slowly a solution of (4-chlorosulfonyl-2-ethyl-phenoxy)-acetic acid ethyl ester (15 g, 48.9 mmol) in glacial acetic acid (20 ml). The reaction mixture was refluxed for 24 h. Water (10 ml) was added carefully and the mixture was refluxed for further 1 h after cooling, the reaction mixture was filtered and the filtrate diluted with water (100 ml). The mixture was extracted with dichloromethane (3×100 ml), and the organic phases were washed with water. After drying the dichloromethane phase was evaporated to give crude (2-ethyl-4-mercapto-phenoxy)-acetic acid in 10 g (96%) yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129268B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-20bc1b6bef784024935ef71c58c9fb54 |
| 出典メモ | uspto-grants-2006_10 |