Hydrazine → 4-Bromopyridazine-3,6-diol
反応式
O.[NH2:2][NH2:3].[Br:4][C:5]1[C:6](O[C:9](=[O:11])[CH:10]=1)=[O:7].NN>C1COCC1>[Br:4][C:5]1[C:6](=[O:7])[NH:2][NH:3][C:9](=[O:11])[CH:10]=1参加物
5
実験手順
Hydrazine hydrate (28 ml, 576 mmol) was added dropwise to a stirred solution of bromomaleic anhydride (100 g, 565 mmol) in THF (1 l) cooled in an ice-bath so that the internal temperature did not exceed 10° C. After complete addition of the hydrazine the mixture was refluxed for 18 h. Solvent was removed by evaporation and the residues were dried by azeotroping with toluene. The residue was triturated and washed with diethyl ether to give the title compound as an orange solid (83 g, 77%). 1H NMR (250 MHz , d6-DMSO) δ 7.68 (1H, br s). MS (ES+) m/e 193 [MH]+, 191 [MH]+. This material was used without further purification.
後処理
- temperaturecooled in an ice-bath so that the internal temperature
- customdid not exceed 10° C
- temperaturewas refluxed for 18 h
- customSolvent was removed by evaporation
- customthe residues were dried
- customby azeotroping with toluene
- customThe residue was triturated
- washwashed with diethyl ether
出典と根拠
- ORDレコード
- ord-d910e63b15bf4e63a4ea8b86dbac71fa
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06303605B1
反応ノート
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