関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Bromobenzyl bromide | HCID 69979 | — |
| 反応物 | 1-Dimethylcarbamoyl-4-(3-trimethylsilyloxypropyl)imidazole | HCID 11277222 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-[(3-bromophenyl)methyl]-1H-imidazole-5-propanol | HCID 15035669 | 100% |
反応手順
A solution of 250 parts of 1-bromo-3-bromomethylbenzene, 168.5 parts of N,N-dimethyl-4-[3-[(trimethylsilyl)oxy]propyl]-1H-imidazole-1-carboxamide and 869 parts of acetonitrile was refluxed for 18 hours. After cooling to 0° C., ammonia was bubbled through the reaction mixture for 5 min. The solvent was evaporated and the residue was stirred for 1 hour in 1700 ml of hydrochloric acid 1N. The mixture was extracted with ethyl acetate. The aqueous layer was basified with Na2CO3 (sat.) and reextracted with ethyl acetate (5×450 parts). The combined extracts were washed with water, dried, filtered and evaporated, yielding 210 parts (100%) of 1-[(3-bromophenyl)methyl]-1H-imidazole-5-propanol (interm. 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05066656 |
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| 出典データセット | uspto-grants-1991_11 |
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| ORD ID | ord-94c0f80aa981442d9037134b965a85be |
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| 出典メモ | uspto-grants-1991_11 |
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