反应 #586140

反应方程式

2-propylthio-4-(3-trifluoromethylpyrazolyl)benzaldehyde

triethylsilane

→

[2-methyl-5-(3-trifluoromethylpyrazolyl)phenyl] propyl sulfide

收率 19.3%

溶剂

methylene chloride

methylene chloride

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   其他The methylene chloride layer was separated
3. 3
   洗涤washed with 30 ml of water twice
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe methylene chloride was distilled off under reduced pressure
6. 6
   其他Purification of the residue by silica gel column chromatography

实验过程

0.98 g (3.1 mmol) of 2-propylthio-4-(3-trifluoromethylpyrazolyl)benzaldehyde (Compound No. V-159 of the present invention) prepared in the same manner as in Example 8 (9) was dissolved in 10 ml of methylene chloride and stirred together with 1.44 g (12.4 mmol) of triethylsilane and 0.63 ml (6.8 mmol) of boron trifluoride diethyl ether complex at room temperature for 22 hours. The reaction mixture was poured into 50 ml of ice-cold water, and 20 ml of methylene chloride was added. The methylene chloride layer was separated, washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the methylene chloride was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 0.18 g of [2-methyl-5-(3-trifluoromethylpyrazolyl)phenyl] propyl sulfide (yield 19.3%) as a colorless liquid (nD20 unmeasurable).

来源