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Stannous Chloride → Ethyl (2-amino-6-methoxy-phenyl)-carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | Ethyl (2-methoxy-6-nitrophenyl)carbamate | HCID 86603972 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Ethyl (2-amino-6-methoxy-phenyl)-carbamate | HCID 86603973 | — |
反応手順
25.0 g (0.104 mol) ethyl (2-methoxy-6-nitro-phenyl)-carbamate are dissolved in 400 mL methanol. 116.4 g (0.516 mol) SnCl2 2H2O are added and the mixture is refluxed for 3 hours. The reaction mixture is evaporated down, combined with sodium carbonate solution and filtered. The aqueous phase is repeatedly extracted with dichloromethane and the combined organic phases are washed with sodium chloride solution, dried and evaporated down. The residue that crystallises out on standing is stirred with isopropanol. Yield: 13.0 g (59%); mass spectroscopy: [M+H]+=211.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429583B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-0b62773a7e51420fbebb818a281d5476 |
| 出典メモ | uspto-grants-2008_09 |