Hydrochloric Acid → ethyl 3-amino-1-methyl-1H-pyrazole-4-carboxylate
反応式
Cl.C(=[N:9][N:10]([CH:12]=[C:13]([C:19]#[N:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH3:11])C1C=CC=CC=1>C(O)C>[NH2:20][C:19]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][N:10]([CH3:11])[N:9]=1参加物
4
実験手順
At room temperature, 100 ml of concentrated hydrochloric acid were added dropwise over a period of 20 min to a suspension of 220 g (0.855 mol) of ethyl 3-(N′-benzylidene-N-methylhydrazino)-2-cyanoacrylate (XVI-1) in 1000 ml of ethanol. The mixture was then heated at the boil for 1 hour. After removal of the solvent, the oily residue was triturated with gentle heating with 200 ml of diethyl ether, resulting in the precipitation of a solid. Filtration with suction gave 149 g (95% of theory) of ethyl 3-amino-1-methyl-1H-pyrazole-4-carboxylate [log P (pH 2.3)=0.72].
後処理
- temperatureThe mixture was then heated at the boil for 1 hour
- customAfter removal of the solvent
- customthe oily residue was triturated
- temperaturewith gentle heating with 200 ml of diethyl ether
- customresulting in the precipitation of a solid
- filtrationFiltration with suction
出典と根拠
- ORDレコード
- ord-ddbd24bdeb3545ac8f1de7a54cf79c6a
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07906656B2
反応ノート
読み込み中…