Hydrazine hydrate (1:1) → 3-(3-Bromo-5-chlorophenoxy)-2-hydrazino-4-methylpyridine
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:14]=[C:15]([Cl:17])[CH:16]=1)[O:5][C:6]1[C:7](Cl)=[N:8][CH:9]=[CH:10][C:11]=1[CH3:12].O.[NH2:19][NH2:20]>CS(C)=O>[Br:1][C:2]1[CH:3]=[C:4]([CH:14]=[C:15]([Cl:17])[CH:16]=1)[O:5][C:6]1[C:7]([NH:19][NH2:20])=[N:8][CH:9]=[CH:10][C:11]=1[CH3:12]参加物
4
反応条件
- 温度
- 100 °C
実験手順
To a solution of 3-(3-bromo-5-chlorophenoxy)-2-chloro-4-methylpyridine (121 mg, 0.363 mmol) in DMSO (1 mL) was added hydrazine hydrate (177 μL, 3.63 mmol) and the mixture was heated at 100° C. for 18 hours. The mixture was then purified on a Luna column (10μ, C18, 250×21.2 cm) eluting with 5-95% ACN/water with 0.1% TFA) to give the title compound. LRMS (M+1)=329.8.
後処理
- customThe mixture was then purified on a Luna column (10μ, C18, 250×21.2 cm)
- washeluting with 5-95% ACN/water with 0.1% TFA)
出典と根拠
- ORDレコード
- ord-74fa4eb2ab544001a16aace5362289d0
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07781454B2
反応ノート
読み込み中…