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Sulfuric acid magnesium salt (1:1) → Ethyl 2-(morpholin-4-yl)-1,3-thiazole-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | Ethyl bromopyruvate | HCID 66144 | — |
| 反応物 | 4-Morpholinecarbothioamide | HCID 2393544 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Ethyl 2-(morpholin-4-yl)-1,3-thiazole-4-carboxylate | HCID 15053544 | 55.2% |
反応手順
A mixture of 1.85 g (12.7 mmol) of 4-((amino)thiocarbonyl)morpholine, 1.59 ml (12.7 mmol) of ethyl bromopyruvate, and excess MgSO4 in 50 ml of acetone was heated at reflux for 2 h. The resulting mixture was allowed to cool, filtered, and concentrated in vacuo. The residue was taken up in chloroform, washed with aqueous NaHCO3, dried over Na2SO4, and concentrated. Silica gel chromatography using 1% methanol in chloroform provided 1.7 g (55%) of the desired compound, Rf 0.70 (ethyl acetate). Mass spectrum: (M+H)+ =243.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05616720 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-fca97fda05a746c180b888f83883c67a |
| 出典メモ | uspto-grants-1997_04 |