Phosphorus oxychloride → Ethyl 3-chloropyridazine-4-carboxylate
反応式
[CH2:1]([O:3][C:4]([C:6]1[C:7](=O)[NH:8][N:9]=[CH:10][CH:11]=1)=[O:5])[CH3:2].O=P(Cl)(Cl)[Cl:15]>>[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][N:9]=[N:8][C:7]=1[Cl:15])=[O:5])[CH3:2]参加物
3
反応条件
- 温度
- 100 °C
実験手順
A mixture of 3-oxo-2,3-dihydro-pyridazine-4-carboxylic acid ethyl ester (355 mg, 2.11 mmol) and POCl3 (6 ml) was heated to 100° C. for 1 h. The volatiles were then removed and the remaining residue was neutralized with sat. NaHCO3-solution. This mixture was extracted three times with Et2O and the combined extracts were dried (Na2SO4) and evaporated to obtain the crude title compound. The remaining brown solid (364 mg, 1.95 mmol, 92%) was used in the next reaction step without further purification. MS: m/e=187.1 [M+H+].
後処理
- customThe volatiles were then removed
- extractionThis mixture was extracted three times with Et2O
- dry with materialthe combined extracts were dried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-d808e1385b484337a713e8cbd1a57e8b
- 出典データセット
- uspto-grants-2011_04
- 特許番号
- US07928106B2
反応ノート
読み込み中…