関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl thiooxamate | HCID 2733398 | — |
| 反応物 | 3-Bromo-1-(3-bromophenyl)butan-2-one | HCID 86711492 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 4-(3-bromobenzyl)-5-methylthiazole-2-carboxylate | HCID 86711493 | — |
反応手順
A mixture of ethyl 2-amino-2-thioxoacetate (50.9 mg, 0.38 mmol) and 3-bromo-1-(3-bromophenyl)butan-2-one (0.38 mmol, crude from previous step) in DMF (2 mL) was stirred at 70° C. for 12 h. The mixture was diluted with EtOAc and washed with H2O. The organic layer was concentrated, and purified by silica gel column chromatography(0-50% EtOAc/Hexane) to yield a yellowish solid (71 mg, 55% over 2 steps). MS (ES+) C14H14BrNO2S requires: 339, 341 found: 340, 342 [M+H]+(1:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09115120B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-5e08d89a8e144122b3b56f9f5521f41a |
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| 出典メモ | uspto-grants-2015_08 |
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