Ammonia → (+/-)-3-(2-Pyridyl)-4,5-dihydro-1-(3-mercapto-1-oxopropyl)-1H-pyrazole-5-carboxylic acid
反応式
N.C([S:5][CH2:6][CH2:7][C:8]([N:10]1[CH:14]([C:15]([OH:17])=[O:16])[CH2:13][C:12]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)=[N:11]1)=[O:9])(=O)C>>[N:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[C:12]1[CH2:13][CH:14]([C:15]([OH:17])=[O:16])[N:10]([C:8](=[O:9])[CH2:7][CH2:6][SH:5])[N:11]=1参加物
3
実験手順
Aqueous ammonia (12 ml of 7 N) is stirred at 0°-5° C. under argon and 3.5 g of (±)-1-[3-(acetylthio)-1-oxopropyl]-3-(2-pyridyl)-4,5-dihydro-1H-pyrazole-5-carboxylic acid is added. The resulting solution is stirred for 2 hours under argon and is then extracted with ethyl acetate (discarded). The aqueous layer is acidified with acetic acid and extracted with ethyl acetate (three 50 ml portions). The combined organic layers are washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to yield the title compound.
後処理
- extractionis then extracted with ethyl acetate (discarded)
- extractionextracted with ethyl acetate (three 50 ml portions)
- washThe combined organic layers are washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-71cc72670eb44bdeabe440da9b22a19b
- 出典データセット
- uspto-grants-1981_03
- 特許番号
- US04254267
反応ノート
読み込み中…