Ethyl orthoformate → 4-Chloro-7-cyclopentyl-7H-imidazo[4,5-c]pyridazine
反応式
[Cl:1][C:2]1[C:3]([NH2:14])=[C:4]([NH:8][CH:9]2[CH2:13][CH2:12][CH2:11][CH2:10]2)[N:5]=[N:6][CH:7]=1.[CH2:15](OC(OCC)OCC)C>>[Cl:1][C:2]1[C:3]2[N:14]=[CH:15][N:8]([CH:9]3[CH2:13][CH2:12][CH2:11][CH2:10]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-cyclopentylpyridazine-3,4-diamine (Preparation 12, 1.2 g, 5.64 mmol) and triethylorthoformate (10 mL) were heated to reflux for 1.5 hours. The reaction mixture was allowed to cool to room temperature, concentrated in vacuo and triturated with EtOAc (20 mL). The solid was filtered and the filtrate was reduced to dryness. The crude material was purified by silica gel column chromatography eluting with EtOAc to afford the title compound as a yellow solid in 51% yield, 902 mg.
後処理
- temperaturewere heated
- temperatureto reflux for 1.5 hours
- concentrationconcentrated in vacuo
- customtriturated with EtOAc (20 mL)
- filtrationThe solid was filtered
- customThe crude material was purified by silica gel column chromatography
- washeluting with EtOAc
出典と根拠
- ORDレコード
- ord-76aa0d6429ff4453a36bf33c1fe2c3c8
- 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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