반응 #90526

반응 방정식

PTSA

13

6-methoxy-5-morpholino-2,3-dihydro-1H-inden-1-one

4-((trifluoromethyl)thio)benzaldehyde

→

crude compound 73

(E)-6-methoxy-5-morpholino-2-(4-((trifluoromethyl)thio)benzylidene)-2,3-dihydro-1H-inden-1-one

용매

ethyl acetate

toluene

반응 조건

후처리

1. 1
   세척washed with water (3×25 mL)
2. 2
   건조The organic layer was dried over sodium sulphate
3. 3
   농축concentrated

실험 절차

To a solution of 13 (1.2 g, 4.858 mmol) in toluene 40 mL was added 4-((trifluoromethyl)thio)benzaldehyde 72 (1 g, 4.858 mmol). PTSA (1.84 g, 9.716 mmol) was added and the reaction mixture was stirred at 120° C. for 6 h. The reaction mass was diluted with ethyl acetate and washed with water (3×25 mL). The organic layer was dried over sodium sulphate and concentrated to get the crude compound 73, which was purified through flash chromatography by using 100-200 mesh silica gel. The compound (E)-6-methoxy-5-morpholino-2-(4-((trifluoromethyl)thio)benzylidene)-2,3-dihydro-1H-inden-1-one 73 was eluted at 37% ethyl acetate in hexane to afford yellow coloured solid.

출처