化工社化工社 化学情報印刷レポート · 研究参考用
ethyl 2-((N-methylsulfamoyl)amino)acetate → 2-Methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | ethyl 2-((N-methylsulfamoyl)amino)acetate | HCID 18449915 | — |
| 反応物 | HCID 178418922 | HCID 178418922 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide | HCID 364077 | 54% |
反応手順
To a solution of ethyl 2-((N-methylsulfamoyl)amino)acetate from the previous step (3.5 mmol) in DMF (50 mL) is added KO-t-Bu (1.56 g, 13.88 mmol) in portions under N2 at RT. The mixture is stirred overnight then quenched with HCl/methanol (2 M). After the solvent is removed in vacuo, the residue is washed with water to afford 2-methyl-1,1-dioxo-1λ6-[1,2,5]thiadiazolidin-3-one (480 mg, 54%). 1H-NMR (CDCl3): δ 7.36 (d, J=8.4 Hz, 2H), 6.87 (d, J=8.8 Hz, 2H), 4.87 (m, 1H), 4.68 (s, 2H), 4.03 (d, J=7.2 Hz, 2H), 3.80 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07202257B2 |
| 出典データセット | uspto-grants-2007_04 |
| ORD ID | ord-eab21331a3d7413b86de1d8f2fe75ba5 |
| 出典メモ | uspto-grants-2007_04 |