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S-Ethylisothiourea → HCID 178477341、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | S-Ethylisothiourea | HCID 5139 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Propenoic acid, 2-cyano-3-ethoxy-, ethyl ester | HCID 78943 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178477341 | HCID 178477341 | 63.6% |
反応手順
To a solution of potassium hydroxide (640 mg, 10 mmol) in methanol (6 mL) at 0° C. was added 2-ethyl-2-thiopseudourea (1.85 g, 10 mmol). The mixture was warmed to room temperature, stirred for 5 min, then filtered off potassium bromide under N2. The filtrate was cooled down to 0° C. then ethyl (ethoxymethylene)cyanoacetate (420 mg, 2.5 mmol) was added. The mixture was gradually warmed to room temperature and stirred for 20 h. The solvent was removed under reduced pressure, and the crude material was purified by flash chromatography using 4% 2M NH3 in MeOH/CH2Cl2 system to obtain 288 mg of the title compound. Mass spectrum 181 (EI, M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06498165B1 |
| 出典データセット | uspto-grants-2002_12 |
| ORD ID | ord-eba92fbec2954e5dbeea0bfa6f37264a |
| 出典メモ | uspto-grants-2002_12 |