関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chlorobenzimidazole | HCID 78572 | — |
| 反応物 | 2-Bromo-1-(4-methoxypyridin-2-yl)ethanone | HCID 19846114 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Isopropyl alcohol isopropyl ether | HCID 21202047 | — |
反応手順
2-Bromoacetyl-4-methoxypyridine (11.5 g, 0.05) and 2-chlorobenzimidazole (7.5 g, 0.05 mole) were dissolved in dimethylformamide (75 ml) and cooled to 2° C. K2CO3 (12 g, 0.08 mole) was added and the temperature rose to 9° C. as the suspension was stirred for 1/2 hour. The mixture was added to H2O (200 ml) giving a solid which was removed by filtration. The mother liquors were extracted with ethyl acetate and the solid was dissolved in the extracts. The organic solution was washed (brine) and dried (MgSO4) and purified by passage down a silica column and evaporated to dryness to give a sticky solid. Trituration with propan-2-ol/di-isopropyl ether gave 2-chloro-1-[2-(2-[4-methoxypyridyl])-2-oxoethyl]-benzimidazole (7.2 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04725605 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-e54381d6a37d4ac89c8f8f5dc9dbc8ea |
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| 出典メモ | uspto-grants-1988_02 |
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