関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromomethyl 4-methoxyphenyl ketone | HCID 4965 | — |
| 反応物 | Thioacetamide | HCID 2723949 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(4-Methoxy-phenyl)-2-methyl-thiazole | HCID 768765 | 69.6% |
反応手順
The mixture of thioacetamide (16.0 g, 213 mmol) and 2-bromo-1-(4-methoxy-phenyl)-ethanone (4.0 g, 17.5 mmol) was heated at 140° C. for 24 h under nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), water (100 mL) was added and extracted with ethyl acetate (3×100 mL). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated. The crude residue was purified over silica gel (230-400 M, 1% EtOAc-Hexane) to get the desired product (2.5 g, 69%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08865736B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-40038c5191d440f58f1034e6dd273126 |
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| 出典メモ | uspto-grants-2014_10 |
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