Sodium Hydroxide → 6-Methyl-4-pyridazinecarboxylic acid hydrochloride
反応式
Cl[C:2]1[N:3]=[N:4][C:5]([CH3:11])=[CH:6][C:7]=1[C:8]([OH:10])=[O:9].[OH-].[Na+]>CO.[Pd]>[CH3:11][C:5]1[N:4]=[N:3][CH:2]=[C:7]([C:8]([OH:10])=[O:9])[CH:6]=1参加物
5
実験手順
To a stirred solution of 3-chloro-6-methyl-pyridazine-4-carboxylic acid (500 mg, 2.89 mmol) in MeOH (50 mL) was added NaOH (395 mg, 9.85 mmol) in pellets, followed by 150 mg of Pd/C (10%). The reaction mixture was put under a H2 atmosphere for 3 hours (atmospheric pressure). The reaction mixture was filtered on celite, acidified with aq. HCl (pH=6), and concentrated under vacuo. Column chromatography (SiO2, CH2Cl2/MeOH 7/3) yielded 6-methyl-pyridazine-4-carboxylic acid (120 mg, 29%) as a brown solid.
後処理
- filtrationThe reaction mixture was filtered on celite
- concentrationconcentrated under vacuo
出典と根拠
- ORDレコード
- ord-21d3e6e20703469f9e332bca55fef9ee
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08318759B2
反応ノート
読み込み中…