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Hydrochloric Acid → HCID 178500931、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Dimethyl 3-oxoglutarate | HCID 74591 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178500931 | HCID 178500931 | — |
反応手順
A mixture of 2.5 ml of concentrated HCl, 5 ml of H2O, and 5.523 mmoles of aniline (26) was treated with a solution of sodium nitrite 381 mg (5.52 mmoles) in 5 ml of water in an ice bath. This reaction was stirred for two hours to give crude diazonium chloride (27) which was not isolated. The crude diazonium salt solution was poured into a mixture of 961 mg of dimethyl acetonedicarboxylate (2) in 3 ml of ethanol and 3 g of sodium acetate in 10 ml of water with vigorous stirring. Product precipitated immediately. The reaction was allowed to stir for an additional 2 hours, then filtered and dried to give 1.363 g of the desired hydrazone (28) as a solid. MS+: m/e=339.1 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653088B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-6ef0804db229450ca0083845d6e32db9 |
| 出典メモ | uspto-grants-2014_02 |