関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thiazole | HCID 9256 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 5-Phenylthiazole | HCID 595209 | — |
反応手順
A solution of thiazole (10.0 g), iodobenzene (2.63 ml), tetrakis(triphenylphosphine)palladium (0) (1.36 g) and potassium acetate (3.46 g) in N,N-dimethylacetamide (100 ml) was stirred under heating at 100° C. overnight. The solvent was evaporated under reduced pressure, and added to the residue was ethyl acetate. The mixture was washed successively with water and brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-90:10) to give 5-phenylthiazole (1.50 g) as a pale yellow solid. APCI-Mass m/Z 162 (M+H). (2) The above 5-phenylthiazole and 5-bromo-2-chlorobenzaldehyde obtained in Reference Example 16-(1) were treated in a manner similar to Reference Example 100 to give 5-bromo-2-chloro-1-(5-phenyl-2-thiazolylmethyl)benzene as a yellow solid. APCI-Mass m/Z 364/366 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08202984B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-bc4a661d554b4a3e914849e6a6bf3ee3 |
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| 出典メモ | uspto-grants-2012_06 |
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