Sodium Acetate → 4-(Piperazin-1-yl)pyridazine
反応式
Cl[C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.C([O-])(=O)C.[Na+]>CO.[Pd]>[N:8]1([C:7]2[CH:6]=[CH:5][N:4]=[N:3][CH:2]=2)[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1参加物
5
実験手順
9.3 g 3,6-dichloro-4-piperazin-1-yl-pyridazine (see 10.2) and 6.5 g sodium acetate are suspended in 100 ml of methanol and hydrogenated with 1 g Pd/C 10% and ambient temperature. The catalyst is suction filtered and the filtrate is evaporated to dryness. The product is extracted with chloroform, washed with sodium hydroxide solution and precipitated as the hydrochloride with an ethereal HCl solution. 8.6 g (V-4) are obtained. M.p>300° C.
後処理
- filtrationfiltered
- customthe filtrate is evaporated to dryness
- extractionThe product is extracted with chloroform
- washwashed with sodium hydroxide solution
- customprecipitated as the hydrochloride with an ethereal HCl solution
- custom8.6 g (V-4) are obtained
- customM.p>300° C.
出典と根拠
- ORDレコード
- ord-b1314ee7cc7a4e4487e547c70944bd0d
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115142B2
反応ノート
読み込み中…