反応 #66377

反応方程式

5-(3-Methoxy-phenyl)-4-pyridin-4-yl-2H-pyrazole-3-thiol

chloroacetaldehyde

→

crude product

収率 93.0%

6-(3-methoxy-phenyl)-7-pyridin-4-yl-2,3-dihydro-pyrazolo[5,1-b]thiazol-3-ol

収率 93.0%

溶媒

ethylacetate

THF water

反応条件

後処理

1. 1
   洗浄washed with saturated aqueous NaHCO3 and brine
2. 2
   乾燥dried over Na2SO4
3. 3
   その他evaporated to dryness

実験手順

5-(3-Methoxy-phenyl)-4-pyridin-4-yl-2H-pyrazole-3-thiol prepared as described in Example 8 (115 mg, 0.406 mmol) was dissolved in a 1:1 THF/water mixture (3 mL). A 55% aqueous solution of chloroacetaldehyde (0.071 mL, 0.609 mmol, 1.5 eq) was added and the mixture was stirred at room temperature for 2 hours. It was then diluted with ethylacetate and washed with saturated aqueous NaHCO3 and brine, dried over Na2SO4 and evaporated to dryness to give 123 mg (93%) of crude product, which was used without further purification in the following step.

出典