반응 #2143802

반응 방정식

NaHCO3

NaHCO3

N-(2,4-dimethoxyphenyl)-4-fluorobenzamide

phosphorus pentasulphide

→

expected product

수율 49.0%

N-(2,4-dimethoxyphenyl)-4-fluorobenzenecarbothioamide

수율 49.0%

용매

1,2-dimethoxyethane

반응 조건

후처리

1. 1
   온도is maintained
2. 2
   추출the product is extracted with 3 times 200 ml of ethyl acetate
3. 3
   세척The combined organic phases are washed with twice 200 ml of a saturated solution of NaCl
4. 4
   건조dried over sodium sulphate
5. 5
   기타The solvents are evaporated off under reduced pressure
6. 6
   기타the residue purified on a silica column (eluent: ethyl acetate/heptane mixture 1:4) in order

실험 절차

11 g (131 mmol; 4 equivalents) of NaHCO3 is added to 9 g (32.7 mmol) of N-(2,4-dimethoxyphenyl)-4-fluorobenzamide dissolved in 350 ml of 1,2-dimethoxyethane. 29 g (65.2 mmol; 2 equivalents) of phosphorus pentasulphide (P2S5) is then added by parts to the reaction medium which is maintained under stirring under an inert atmosphere of argon at 85° C. for 4 hours. 250 ml of a saturated solution of NaHCO3 are then added to the medium then the product is extracted with 3 times 200 ml of ethyl acetate. The combined organic phases are washed with twice 200 ml of a saturated solution of NaCl, then dried over sodium sulphate. The solvents are evaporated off under reduced pressure and the residue purified on a silica column (eluent: ethyl acetate/heptane mixture 1:4) in order to provide 4.65 g (yield=49%) of expected product.

출처