関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphinic Acid | HCID 4124402 | — |
| 反応物 | (Rac)-1-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-1-(imidazo[1,2-a]pyridin-6-yl)ethanol | HCID 87523871 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 57917275 | HCID 57917275 | — |
反応手順
Iodine (4.8 g, 18.91 mmol) and H3PO2 (5.1 mL of a 50% aqueous solution, 46.8 mmol) were added to a solution of (rac)-1-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-1-(imidazo[1,2-a]pyridin-6-yl)ethanol (Stage 292.1, 1.85 g, 5.90 mmol) in acetic acid (50 mL). The RM was portion wise in 3 different microwave reactors and was heated at 150° C. for 5 min under microwave irradiations. It was basified with 2.5 N NaOH solution and then it was extracted twice with EtOAc/MeOH (9:1) twice. Combined organic layers was washed with brine and dried over Na2SO4, filtered and concentrated to give the title compound as a brown solid (tR 0.5 min (conditions 2), MH+=298)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822468B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-d015060e79b54a65b317e2272ad33c27 |
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| 出典メモ | uspto-grants-2014_09 |
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