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Water → 2-(1,2-Benzoxazol-3-yl)acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydroxylamine, sulfate (1:1) | HCID 159255 | — |
| 反応物 | 4-Hydroxycoumarin | HCID 54682930 | — |
| 触媒 | Edta disodium | HCID 44120005 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 2-(1,2-Benzoxazol-3-yl)acetic acid | HCID 301729 | — |
反応手順
A mixture of hydroxylamine sulfate (344.0 g), water (904 ml) and a 25% aqueous sodium hydroxide solution (456 ml) is stirred, and thereto are added 4-hydroxycoumarin (168.0 g) and ethylenediaminetetraacetic acid disodium salt dihydrate (3.2 g), and the mixture is stirred with heating at 84° C.-86° C. for 4 hours. The reaction mixture is cooled, and thereto is added 1,2-dichloroethane (240 ml). The mixture is stirred, and the aqueous layer is collected. The pH value of the aqueous layer is adjusted to pH 1-2 with 25% sulfuric acid, and the precipitated crystals are collected by filtration, washed with water, and dried with air at 60° C. for 15 hours to give 1,2-benzisoxazole-3-acetic acid (170.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07262304B2 |
| 出典データセット | uspto-grants-2007_08 |
| ORD ID | ord-aad2945f10194c0d86862b7871db640d |
| 出典メモ | uspto-grants-2007_08 |