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Hydrochloric Acid → 4-Bromoisoquinolin-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 4-Bromo-5-nitroisoquinoline | HCID 271280 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Bromoisoquinolin-5-amine | HCID 14580057 | — |
反応手順
100 ml of concentrated hydrochloric acid are added to a suspension of 16 g of the compound obtained in Step 1 in 55 ml of ethanol. The mixture is cooled with ice and stirred whilst a solution of 62.6 g of SnCl2.2H2O in 100 ml of ethanol is being introduced and then for a further 3 hours. After removal of the solvent by evaporation, the residue is diluted with 140 ml of ice-cold water and rendered basic with 2N sodium hydroxide solution. The resulting aqueous phase is extracted 3 times with 350 ml of methylene chloride each time. The combined organic phases are dried over MgSO4 and evaporated. The residue is purified by flash chromatography (CH2Cl2/MeOH: 98/2) to yield the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06323217B2 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-e8ca5b4f452b4f1d8ea5c2c01c666ed8 |
| 出典メモ | uspto-grants-2001_11 |