関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 1-Phenethylamine, (-)- | HCID 75818 | — |
| 反応物 | 2-(4-Fluorophenyl)-1-(2-methylthio-4-pyrimidinyl)-5-aminoimidazo[4,5-b]pyridine | HCID 22486130 | — |
| 溶媒 | Acetic acid methylene chloride | HCID 21922555 | — |
| 生成物 | 2-(4-Fluorophenyl)-1-(2-(1-(S)-phenylethyl)amino-4-primidinyl)-5-aminoimidazo[4,5-b]pyridine | HCID 9845305 | 52% |
反応手順
2-(4-Fluorophenyl)-1-(2-methylthio-4-pyrimidinyl)-5-aminoimidazo[4,5-b]pyridine (110 mg, 0.31 mmol) is dissolved in CH2Cl2/HOAc 1:1 (6.2 ml), combined at 0° C. with mCPBA (84 mg 70% 0.34 mmol) and stirred for 30 min. The reaction mixture is poured on 2N Na2CO3 and extracted with ethyl acetate three times. The combined organic phases are dried over Na2SO4, filtered and evaporated to dryness to yield the crude sulfoxide (110 mg). 50 mg are dissolved in 1-(S)-phenylethylamine (0.5 ml) and heated to 120° C. for 1 h. Purification over RP18 (CH3CN/Water 70/30 to 10/90) yielded the title compound as light brown foam (30 mg 52%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06608072B1 |
|---|
| 出典データセット | uspto-grants-2003_08 |
|---|
| ORD ID | ord-e0517b94d44b489cb932683350041fdf |
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| 出典メモ | uspto-grants-2003_08 |
|---|
