반응 #931

반응 방정식

water

2,6-dinitrobenzonitrile

K2CO3

3,5-dimethylthiophenol

→

2-[(3,5-dimethylphenyl)thio]-6-nitrobenzonitrile

용매

DMF

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring an additional 30 min
2. 2
   workup.STIRRINGstirred for 1 hr
3. 3
   여과The solid was collected by vacuum filtration

실험 절차

A mixture of 2,6-dinitrobenzonitrile (1.4 g 7.2 mmol) and K2CO3 (1.1 g, 7.9 mmol) in 10 ml of DMF was chilled to 0° C. A solution of 3,5-dimethylthiophenol (1.1 g 0.0079 mmol) in 10 ml of DMF, was added dropwise over 30 min with stirring under nitrogen. After stirring an additional 30 min, the reaction mixture was poured into 150 ml of water and stirred for 1 hr. The solid was collected by vacuum filtration. Chromatography on silica gel (flash; Hex/EtOAc 1:1) provided 1.64 g (80%) of 2-[(3,5-dimethylphenyl)thio]-6-nitrobenzonitrile: mp 155°-156° C.

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