関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Magnesium Carbonate | HCID 11029 | — |
| 反応物 | Chloromalonaldehyde | HCID 147646 | — |
| 反応物 | tert-butyl N-[(1S)-1-carbamothioylethyl]carbamate | HCID 10932591 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Tert-butyl 1-(5-formylthiazol-2-yl)ethylcarbamate | HCID 86657335 | 71.5% |
反応手順
A mixture of (S)-tert-butyl 1-amino-1-thioxopropan-2-ylcarbamate (6.9 g, 0.03 mol), 2-chloromalonaldehyde (5.2 g, 0.049 mol) and magnesium carbonate (2.76 g, 0.03 mol) in 1,4-dioxane (400 mL) was heated at 60° C. for 3 hours and further at room temperature overnight. The reaction mixture was concentrated and the residue purified by column chromatography (50-80% EtOAc/hexane) to afford tert-butyl 1-(5-formylthiazol-2-yl)ethylcarbamate (5.5 g, 64%). LC-MS: (FA) ES+ 257.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09227951B2 |
|---|
| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-f7575ef37cc1429288f17fcac56035ab |
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| 出典メモ | uspto-grants-2016_01 |
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