関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Dichloroacetone | HCID 10793 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Thiophenecarboxamide | HCID 22063 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(Chloromethyl)-2-(thiophen-2-yl)-1,3-oxazole | HCID 2529531 | 57% |
反応手順
A mixture of 2-thiophenecarboxamide (5.09 g) and 1,3-dichloroacetone (457 g) was stirred at 120° C. for 2 hours. The reaction mixture was poured into water, nautralized with potassium carbonate, and then extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography. From the fraction eluted with diethyl ether-hexane (1:9, v/v), 4-chloromethyl-2-(2-thienyl)oxazole (4.09 g, 57%) was obtained. Recrystallization from isopropylether gave colorless needles, mp 59-59° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211215B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-c0f2cf7c7df84db1a690d728e4081640 |
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| 出典メモ | uspto-grants-2001_04 |
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