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Hydrochloric Acid → 2-Hydroxyimino-N-indan-5-yl-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chloral Hydrate | HCID 2707 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Indan-5-amine | HCID 90496 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Hydroxyimino-N-indan-5-yl-acetamide | HCID 72282005 | 60% |
反応手順
This compound is prepared according to the process described in Organic Syntheses, 1925, V, 71-74. A solution of 16.5 ml of concentrated HCl in 120 ml of water and a solution of 41.5 g of hydroxylamine hydrochloride in 70 ml of water are added to a mixture of 25 g of 5-aminoindane, 35 g of chloral hydrate and 22 g of Na2SO4 in 600 ml of water, and the mixture is then refluxed for 30 minutes. After cooling the reaction mixture to RT, it is extracted with EtOAc, the organic phase is dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is taken up in a pentane/iso ether mixture and the precipitate formed is spin-filtered off. 23 g of the expected product are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425566B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-2870f34e8b1c47c59fdc29725e9d888c |
| 出典メモ | uspto-grants-2008_09 |