化工社化工社 化学情報印刷レポート · 研究参考用
N,N'-Dimethylethylenediamine → ethyl 3-[4-(4-ethylphenyl)-1H-1,2,3-triazol-1-yl]benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 1-Ethyl-4-ethynylbenzene | HCID 142425 | — |
| 反応物 | Ethyl 3-iodobenzoate | HCID 143542 | — |
| 反応物 | Sodium Ascorbate | HCID 23667548 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | (Methanesulfinyl)methane--water (1/1) | HCID 23503278 | — |
| 生成物 | ethyl 3-[4-(4-ethylphenyl)-1H-1,2,3-triazol-1-yl]benzoate | HCID 67030215 | — |
反応手順
A mixture of ethyl 3-iodobenzoate (4-1) (138 mg, 0.5 mmol), sodium azide (34 mg, 0.52 mmol), 1-ethyl-4-ethynylbenzene (4-2) (65 mg, 0.5 mmol), CuI (10 mg), MeNHCH2CH2NHMe (11 μL), sodium ascorbate (10 mg), DMSO-H2O (v/v 5:1, 1.5 mL) is stirred at room temperature for 2 hours. The reaction mixture is then poured into ethyl acetate (50 mL), washed with water (10 mL) and brine (10 mL), dried over Na2SO4, filtered and evaporated. The residue is purified on silica gel (0-33% ethyl acetate in hexane) to give ethyl 3-[4-(4-ethylphenyl)-1H-1,2,3-triazol-1-yl]benzoate as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08362050B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-04d8a6fc35784539b2a7b23ce7e955f3 |
| 出典メモ | uspto-grants-2013_01 |