関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Dithionite | HCID 24489 | — |
| 反応物 | Tert-butyl [4-(7-bromo-3-nitroquinolin-4-ylamino)butyl]carbamate | HCID 21984414 | — |
| 触媒 | 1,1'-Diethyl-4,4'-bipyridinium dibromide | HCID 11474262 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tert-butyl [4-(3-amino-7-bromoquinolin-4-ylamino)butyl]carbamate | HCID 21984174 | 99% |
反応手順
A solution of sodium hydrosulfite (43.35 g, 249 mmol) and potassium carbonate (38.28 g, 277 mmol) in water (300 mL) was added to a mixture of tert-butyl[4-(7-bromo-3-nitroquinolin-4-ylamino)butyl]carbamate (24.3 g, 55.3 mmol) and 1,1′-diethyl-4,4′-bipyridinium dibromide (1.03 g, 2.76 mmol) in dichloromethane (368 mL) and water (40 mL), and the reaction was stirred overnight at ambient temperature. The reaction mixture was filtered through a layer of CELITE filter aid. The aqueous filtrate was extracted with dichloromethane, and the combined organic fractions were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to provide 22.4 g of tert-butyl[4-(3-amino-7-bromoquinolin-4-ylamino)butyl]carbamate as a brown powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091214B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-ab593658aea3483d87d1ad57cc97e475 |
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| 出典メモ | uspto-grants-2006_08 |
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