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Hydrazine hydrate (1:1) → HCID 178518884、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 5-Bromo-3-hydroxyisoindolin-1-one | HCID 11615537 | — |
| 生成物 | HCID 178518884 | HCID 178518884 | 95.4% |
反応手順
A mixture of 5-bromo-3-hydroxyisoindolin-1-one (16, 17.0 g, 75 mmol), and hydrazine, monohydrate (60 mL, 1193 mmol) was stirred at room temperature for 15 h, after which a white solid precipitated out (M+1=225, 227). The mixture was diluted with 100 mL H2O, neutralized with conc. HCl to a PH of about 7. The precipitate was filtrated and washed with 100 mL H2O. The solid was collected, azeotropically dried with toluene (3×50 mL) and further dried in a vacuum oven at 45° C. for 15 h, to yield 6-bromophthalazin-1-ol 17 (16.1 g). Found MS (ES+): 225, 227 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08101612B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-a017898196dc48e88a230e2478545716 |
| 出典メモ | uspto-grants-2012_01 |