化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → 6-(2-{1-[5-(3,4-Dichlorophenyl)-4-hydroxythiophen-3-yl]ethylidene}hydrazinecarbothioamido)-2,3-dihydrobenzo[1,4]dioxine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,3-Dihydro-1,4-benzodioxin-6-yl isothiocyanate | HCID 2776173 | — |
| 反応物 | 2-(3,4-Dichlorophenyl)-4-(1-hydrazinylideneethyl)thiophene-3-ol | HCID 71405258 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(2-{1-[5-(3,4-Dichlorophenyl)-4-hydroxythiophen-3-yl]ethylidene}hydrazinecarbothioamido)-2,3-dihydrobenzo[1,4]dioxine | HCID 73299958 | 65% |
反応手順
2-(3,4-Dichlorophenyl)-4-(1-hydrazonoethyl)-thiophen-3-ol (25 mg, 0.08 mmol) prepared in Reference Synthetic Example 13 in dimethylformamide (0.25 mL) was stirred with 6-isothiocyanato-2,3-dihydrobenzo[1,4]dioxine (24 mg, 0.13 mmol, at 30° C. for 4 hours. Methanol and water were added to the reaction solution, and the resulting crystals were collected by filtration, washed and dried to give 28 mg of the desired product (yield 65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08134013B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-9fc6e5d3ea8c48748f42dc337b9e83c2 |
| 出典メモ | uspto-grants-2012_03 |