関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Benzyl-1H-benzimidazole | HCID 563347 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Benzylbenzimidazole-2-carboxylic acid | HCID 20068874 | 80% |
反応手順
A solution of 2.08 g (10 mmol) of 1-benzylbenzimidazole in 200 ml of dry tetrahydrofuran was cooled under N2 atmosphere to -78° C. and treated with 8.0 ml (20 mmol) of n-butyllithium. The resulting solution was warmed to 0° C. for 0.5 h, recooled to -78° C., and poured into a mixture of excess dry ice in 200 ml of tetrahydrofuran. After being allowed to warm, the solution was treated with 200 ml of water, washed with ether, neutralized, and washed with ether. The aqueous layer was concentrated in vacuo, after which the residue was triturated with 2% methanol in chloroform and filtered. The filtrate was dried over MgSO4 and concentrated to give 2.01 g (80%) of the desired compound as a white powder. Mass spectrum: (M-OH)+ =235.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04994477 |
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| 出典データセット | uspto-grants-1991_02 |
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| ORD ID | ord-750c5365c4094d608c2b9ce6794daa31 |
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| 出典メモ | uspto-grants-1991_02 |
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