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Diisopropylethylamine → (4-Methoxy-phenyl)-[5-(4-methoxy-phenyl)thiazol-2-yl]-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-Thioureidoanisole | HCID 667549 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 反応物 | [5-(4-Methoxy-phenyl)-thiazol-2-yl]-[4-(2-pyrrolidin-1-yl-ethoxy)-phenyl]-amine | HCID 11188635 | — |
| 生成物 | (4-Methoxy-phenyl)-[5-(4-methoxy-phenyl)thiazol-2-yl]-amine | HCID 11266955 | — |
反応手順
The title compound is prepared as described in Example 3 for [5-(4-methoxy-phenyl)-thiazol-2-yl]-[4-(2-pyrrolidin-1-yl-ethoxy)-phenyl]-amine but using (4-methoxy-phenyl)-thiourea. After addition of the thiourea and subsequent heating to reflux, the reaction mixture is allowed to cool to RT. DIEA (2.0 equiv) is added and the resulting mixture is heated to reflux for 70 min. Purification of the crude product by silica gel (40 g) column chromatography (CH2Cl2/Et2O, 95/5) affords the title compound as a beige solid: ES-MS: 312.9 [M+H]+; single peak at tR=7.66 min (System 1); Rf=0.11 (CH2Cl2/MeOH, 95/5).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07795288B2 |
| 出典データセット | uspto-grants-2010_09 |
| ORD ID | ord-334cbc4250d34130b05740b1826aca95 |
| 出典メモ | uspto-grants-2010_09 |