関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylbarbituric acid | HCID 69860 | — |
| 反応物 | 1-[2-(4-Allyloxy-benzyloxy)-ethyl]-1H-[1,2,3]triazole | HCID 23614530 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(2-[1,2,3]Triazol-1-yl-ethoxymethyl)-phenol | HCID 21075895 | 59% |
反応手順
A solution of 500 mg (1.93 mmol) 1-[2-(4-allyloxy-benzyloxy)-ethyl]-1H-[1,2,3]-triazole in 10 ml dichloromethane was added to a solution of 904 mg (5.79 mmol) 1,3-dimethylbarbituric acid and 58 mg (0.05 mmol) Pd(PPh3)4 in 20 ml dichloromethane and stirred for 4.5 h at 40° C. The mixture was extracted with 3×20 ml sat. NaHCO3-solution and 8 ml water and the combined aqueous phases were reextracted with 2×10 ml dichloromethane. The organic extracts were combined and dried over MgSO4. Solvents were distilled off and the residue purified by chromatography on silica gel (ethyl acetate) to yield 248 mg (59%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429605B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-16c37bc72604453e908e00c60aa3887d |
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| 出典メモ | uspto-grants-2008_09 |
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