反応 #72955

反応方程式

1-tritylpyrazolo[5,4-b]pyridine-4-carbothioamide

3-bromo-1-methyl-2-oxo-cyclohexane-1-carbonitrile

THF

→

4-methyl-2-(1H-pyrazolo[3,4-b]pyridin-4-yl)-4,5,6,7-tetrahydrobenzo[d]thiazole-4-carbonitrile

収率 39.0%

溶媒

EtOH

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated in vacuo
2. 2
   その他purified by column chromatography (70:9:1 DCM/MeOH/NH4OH)
3. 3
   その他to give a white solid
4. 4
   その他after precipitation (67 mg, 39% Yield)

実験手順

A solution of 1-tritylpyrazolo[5,4-b]pyridine-4-carbothioamide (220 mg, 0.5232 mmol) and 3-bromo-1-methyl-2-oxo-cyclohexane-1-carbonitrile (125.0 mg, 0.5785 mmol) in EtOH (10 mL)/THF (1.5 mL) was heated at 90° C. overnight under nitrogen. The reaction mixture was concentrated in vacuo and purified by column chromatography (70:9:1 DCM/MeOH/NH4OH) to give a white solid after precipitation (67 mg, 39% Yield). MS (ES+) 296.08

出典