反応 #329351

反応方程式

4-fluoro-3-chlorophenylthiourea

1,3-dichloroacetone

compound

2′-Amino-6-(2-hydroxyethoxy)-6′-mercapto-3,4′-bipyridine-3′,5′-dicarbonitrile

sodium bicarbonate

→

2′-Amino-6′-[({2-[(3-chloro-4-fluorophenyl)amino]-1,3-thiazol-4-yl}methyl)thio]-6-(2-hydroxyethoxy)-3,4′-bipyridine-3′,5′-dicarbonitrile

溶媒

DMF

反応条件

後処理

1. 1
   温度After cooling
2. 2
   workup.STIRRINGthe mixture is stirred at RT for a further 20 h
3. 3
   ろ過The mixture is then filtered through a paper
4. 4
   ろ過filter
5. 5
   workup.ADDITIONsat. sodium bicarbonate solution (5 ml) is added to the filtrate
6. 6
   抽出The aqueous phase is extracted with ethyl acetate (three times, 5 ml each)
7. 7
   乾燥The combined organic phases are dried over sodium sulphate
8. 8
   その他the solvent is removed on a rotary evaporator

実験手順

209 mg (0.67 mmol) of 4-fluoro-3-chlorophenylthiourea and 89 mg (0.70 mmol) of 1,3-dichloroacetone are dissolved in 5 ml of DMF, and the reaction solution is stirred at 80° C. for 3 h. After cooling, 209 mg (0.67 mmol) of the compound from example 2A and 224 mg (2.67 mmol) of sodium bicarbonate are added, and the mixture is stirred at RT for a further 20 h. The mixture is then filtered through a paper filter, and sat. sodium bicarbonate solution (5 ml) is added to the filtrate. The aqueous phase is extracted with ethyl acetate (three times, 5 ml each). The combined organic phases are dried over sodium sulphate, and the solvent is removed on a rotary evaporator.

出典