関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-[2-(Isobutylamino)benzylthio]imidazo[4,5-b]pyridine | HCID 14839437 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-[2-(Isobutylamino)benzylsulfinyl]imidazo[4,5-b]pyridine | HCID 14839438 | — |
反応手順
In 20 ml of chloroform was dissolved 900 mg of 2-[2-(isobutylamino)benzylthio]imidazo[4,5-b]pyridine. To the resulting solution was portionwise added under chilling with ice 618 mg of m-chloroperbenzoic acid (purity: 80%) over a period of 30 min. To the mixture was added a saturated NaHCO3 solution, and the resulting mixture was then stirred. The organic phase was separated and extracted successively with 20 ml of 0.1N NaOH and 10 ml of 0.1N NaOH. The alkaline extracts were combined and neutralized by NH4Cl, and the deposited oil was extracted with chloroform. The chloroform extract was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate and placed under reduced pressure to distill off the solvent. The residue was crystallized by addition of diethyl ether. The crystalline product was washed with diethyl ether to give 195 mg of 2-[2-(isobutylamino)benzylsulfinyl]imidazo[4,5-b]pyridine as a pale yellow crystalline powder. m.p.: 116° C. (decompn.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04933458 |
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| 出典データセット | uspto-grants-1990_06 |
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| ORD ID | ord-c3c599e2d6d74f9aaa00d14dd2451530 |
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| 出典メモ | uspto-grants-1990_06 |
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