반응 #10033

반응 방정식

N-methylformanilide

butyl vinyl ether

bis-trichloromethylcarbonate

sodium hydroxide

→

N-methyl-N-phenylaminoacrolein

용매

clorobenzene

clorobenzene

반응 조건

후처리

1. 1
   온도The mixture is cooled at about 5° C.
2. 2
   기타After separation of the phases
3. 3
   추출the aqueous layer is extracted with chlorobenzene (90 ml)
4. 4
   세척the combined organic layers are washed with water (100 ml)
5. 5
   기타evaporated under reduced pressure
6. 6
   workup.ADDITIONThe obtained residue (116.9 g, containing, according to HPLC assay, 104.8 g of pure product, 88% molar yield)
7. 7
   기타is used for the next step of the synthesis without any further purification

실험 절차

To a solution of N-methylformanilide (100 g), butyl vinyl ether (74.12 g) in 85 ml of clorobenzene under stirring at 5° C., a solution of bis-trichloromethylcarbonate (87.84 g) in 170 ml of clorobenzene is added dropwise in 2 hours. The reaction mixture is kept under stirring at room temperature overnight. The mixture is cooled at about 5° C. and the pH is corrected to about 7 by adding sodium hydroxide 15% aqueous solution (348 ml). After separation of the phases, the aqueous layer is extracted with chlorobenzene (90 ml) and the combined organic layers are washed with water (100 ml) and evaporated under reduced pressure. The obtained residue (116.9 g, containing, according to HPLC assay, 104.8 g of pure product, 88% molar yield) is used for the next step of the synthesis without any further purification.

출처