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Phloroglucinol → 3-Methyl-2-nitro-butyric acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phloroglucinol | HCID 359 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 反応物 | Ethyl 2-iodo-3-methylbutanoate | HCID 57436974 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Methyl-2-nitro-butyric acid ethyl ester | HCID 13140446 | — |
反応手順
To an ice cooled solution of 5.31 g sodium nitrite and 8 g dried phloroglucinol in 70 ml dimethyl formamide is added a solution of 11.3 g 2-iodo-3-methyl-butyric acid ethyl ester in 30 ml dimethyl formamide. The solution is allowed to warm up to room temperature and is stirred over night. The solvent is removed at reduced pressure. The residue is dissolved in ethyl acetate and washed with water. The organic layer is dried and the solvent is removed. The title compound is obtained as an oil. MS: m/z (M+)=176.1
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530493B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-5d6e3ec387d34890bc6beb155f34c05e |
| 出典メモ | uspto-grants-2013_09 |