関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfamic Acid | HCID 5987 | — |
| 反応物 | 2-(4-Iodophenyl)propanal | HCID 23333829 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 反応物 | Sodium Chlorite | HCID 23668197 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(4-Iodophenyl)propanoic acid | HCID 15225573 | 94.2% |
反応手順
To a solution of 34 g of 2-(4-iodophenyl)propionaldehyde in 100 ml of ethylene chloride was added a solution of 16.5 g of sulfamic acid in 85 ml of water. To the mixture was added dropwise with stirring a solution of 15.2 g of sodium chlorite in 22 ml of water, while maintaining the temperature at 10° to 15° C. After stirring for 10 minutes, about 15 g of sodium hydrogensulfite was added in small portions to the mixture. The organic layer was separated, washed with water, and mixed with 150 ml of 1 N sodium hydroxide solution. The aqueous layer was separated and adjusted to pH 3.0 with 6 N hydrochloric acid to precipitate white crystals. The crystals were collected by filtration, washed with water, and dried to obtain 34 g (94% yield) of 2-(4-iodophenyl)propionic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04230719 |
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| 出典データセット | uspto-grants-1980_10 |
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| ORD ID | ord-df16276f14824d189c533c6068590210 |
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| 出典メモ | uspto-grants-1980_10 |
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