Trichloroisocyanuric Acid → 3-Chloro-6-(chloromethyl)pyridazine
反応式
[Cl:1]N1C(=O)N(Cl)C(=O)N(Cl)C1=O.[Cl:13][C:14]1[N:15]=[N:16][C:17]([CH3:20])=[CH:18][CH:19]=1>C(Cl)(Cl)Cl>[Cl:13][C:14]1[N:15]=[N:16][C:17]([CH2:20][Cl:1])=[CH:18][CH:19]=1参加物
4
反応条件
- 温度
- 60 °C
実験手順
Trichloroisocyanuric acid (3.62 g) was added to a solution of 3-chloro-6-methyl-pyridazine (5.00 g) in chloroform (130 mL) heated to 60° C. The mixture was stirred at 60° C. for 2 h and then at room temperature overnight. The mixture was filtered over Celite and the filtrate was concentrated. The residue was chromatographed on silica gel (cyclohexane/ethyl acetate 98:2→70:30) to give the title compound as a colorless oil that solidified on standing. Yield: 2.48 g (39% of theory); Mass spectrum (ESI+): m/z=163/165/167 (2 Cl) [M+H]+.
後処理
- customat room temperature
- customovernight
- filtrationThe mixture was filtered over Celite
- concentrationthe filtrate was concentrated
- customThe residue was chromatographed on silica gel (cyclohexane/ethyl acetate 98:2→70:30)
出典と根拠
- ORDレコード
- ord-f4bf91a3abab481b9a3af07e8b682cc3
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09090605B2
反応ノート
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