関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Potassium Chlorate | HCID 6426889 | — |
| 反応物 | HCID 178464036 | HCID 178464036 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | HCID 178464037 | HCID 178464037 | — |
反応手順
15 grams of 1-(2-diethylaminoethyl)-2-hydroxy-6-chloro-7-aza-benzimidazole were dissolved in 200 ml of concentrated hydrochloric acid and there were added in portions with stirring 24.5 grams of potassium chlorate at room temperature. The temperature increased temporarily to 33° C. The mixture was stirred for another hour, made alkaline with sodium hydroxide, the mixture extracted with shaking with n-butanol, the extract evaporated in a vacuum and the residue chromatographed over silica gel. The reaction product was recrystallized from ethyl acetate. M.P. 137°-139° C.; Yield: 3 grams.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04247556 |
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| 出典データセット | uspto-grants-1981_01 |
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| ORD ID | ord-b3af77507a9447b2b79d28e48f76a33f |
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| 出典メモ | uspto-grants-1981_01 |
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