Ethyl orthoformate → 4-Chloro-7-cyclopropyl-7H-imidazo[4,5-c]pyridazine
反応式
[Cl:1][C:2]1[C:3]([NH2:12])=[C:4]([NH:8][CH:9]2[CH2:11][CH2:10]2)[N:5]=[N:6][CH:7]=1.[CH2:13](OC(OCC)OCC)C>>[Cl:1][C:2]1[C:3]2[N:12]=[CH:13][N:8]([CH:9]3[CH2:10][CH2:11]3)[C:4]=2[N:5]=[N:6][CH:7]=1参加物
3
実験手順
A mixture of 5-chloro-N-3-cyclopropylpyridazine-3,4-diamine (Preparation 90, 10.0 g, 54 mmol) and triethylorthoformate (120 mL) were heated to reflux for 3 hours. The reaction mixture was concentrated in vacuo and the residue was purified by silica gel column chromatography eluting with CH2Cl2:MeOH 98:2 to afford the title compound as a brown solid in 48% yield, 5 g.
後処理
- temperaturewere heated
- temperatureto reflux for 3 hours
- concentrationThe reaction mixture was concentrated in vacuo
- customthe residue was purified by silica gel column chromatography
- washeluting with CH2Cl2:MeOH 98:2
出典と根拠
- ORDレコード
- ord-0a0fbb9b55924b23a84bb909be399f6b
- 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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