化工社化工社 化学情報印刷レポート · 研究参考用
Water → 5-(4-Hydroxy-benzylidene)-3-(1-methyl-cyclohexylmethyl)-thiazolidine-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-((4-Hydroxyphenyl)methylene)-2,4-thiazolidinedione | HCID 517822 | — |
| 反応物 | (1-Methylcyclohexyl)methyl trifluoromethanesulfonate | HCID 24827766 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-(4-Hydroxy-benzylidene)-3-(1-methyl-cyclohexylmethyl)-thiazolidine-2,4-dione | HCID 74326904 | 42% |
反応手順
A solution of compound vii (0.5 mmol), compound iii (0.6 mmol) and K2CO3 (0.65 mmol) were stirred in DMF (3 mL) at 80° C. for 4 hr, poured into water, extracted with ethyl acetate (3×10 mL), dried and concentrated. The residue was purified by chromatography, affording compound 9 in 42% yield. 1H NMR (300 MHz, CDCl3) δ 0.94 (s, 3H), 1.14-1.86 (m, 10H), 3.63 (s, 2H), 5.69 (s, 1H), 6.94 (d, J=8.40 Hz, 2H), 7.43 (d, J=8.40 Hz, 2H), 7.83 (s, 1H); HRMS exact mass of (M+Na)+, 354.1140 amu; observed mass of (M+Na)+, 354.1141 amu.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07973062B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-e1a6e959fcfb453ab5f9771eaf39757e |
| 出典メモ | uspto-grants-2011_07 |