Ethyl orthoformate → 4-chloro-7-ethyl-7H-imidazo(4,5-c)pyridazine
反応式
[Cl:1][C:2]1[C:3]([NH2:11])=[C:4]([NH:8][CH2:9][CH3:10])[N:5]=[N:6][CH:7]=1.[CH2:12](OC(OCC)OCC)C>>[Cl:1][C:2]1[C:3]2[N:11]=[CH:12][N:8]([CH2:9][CH3:10])[C:4]=2[N:5]=[N:6][CH:7]=1参加物
3
実験手順
A mixture of 5-chloro-N3-ethyl-pyridazine-3,4-diamine (Preparation 7, 10.0 g, 58 mmol) and triethylorthoformate (60 mL) were heated to reflux for 4 hours. The reaction mixture was concentrated in vacuo and the residue was dissolved in EtOAc (50 mL) and filtered. The filter cake was washed with EtOAc and then the organic layers were washed with saturated brine solution, dried over Na2SO4 and concentrated in vacuo to afford the title compound as a yellow solid in 45% yield, 4.8 g.
後処理
- temperaturewere heated
- temperatureto reflux for 4 hours
- concentrationThe reaction mixture was concentrated in vacuo
- dissolutionthe residue was dissolved in EtOAc (50 mL)
- filtrationfiltered
- washThe filter cake was washed with EtOAc
- washthe organic layers were washed with saturated brine solution
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-9682482d34b54dac85b63bf0e39d2623
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08952008B2
反応ノート
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