Water → 4-bromo-2H-phthalazin-1-one
反応式
[C:1]([NH:13][NH2:14])(=O)[C:2]1[C:3](=[CH:8][CH:9]=[CH:10][CH:11]=1)[C:4](NN)=[O:5].P(Br)(Br)(Br)(Br)[Br:16].O>C(Br)(Br)(Br)Br>[Br:16][C:1]1[C:2]2[C:3](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:4](=[O:5])[NH:14][N:13]=1参加物
5
実験手順
A mixture of phthalhydrazide (3.2 g) and phosphorus pentabromide (19.0 g) was heated with stirring in carbon tetrabromide (50 g) at 125° for 16 hours. The cooled mixture was poured into water (50 cm3) and the product collected by filtration. The solid product was chromatographed on silica (Merck "MK 60.9385" [Trade Mark]) eluting with diethyl ether:dichloromethane, 1:3 by volume. Combination and evaporation of appropriate fractions afforded the title compound, m.p. 268°-271° (1.5 g).
後処理
- temperaturewas heated
- filtrationthe product collected by filtration
- customThe solid product was chromatographed on silica (Merck "MK 60.9385" [Trade Mark])
- washeluting with diethyl ether
- customCombination and evaporation of appropriate fractions
出典と根拠
- ORDレコード
- ord-b862737d7f5149f48b00d895c9b4d79c
- 出典データセット
- uspto-grants-1990_02
- 特許番号
- US04898872
反応ノート
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