反応 #90523

反応方程式

PTSA

13

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

3-(trifluoromethyl) picolinaldehyde

→

(E)-6-methoxy-5-morpholino-2-((3-(trifluoromethyl)pyridin-2-yl)methylene)-2,3-dihydro-1H-inden-1-one

溶媒

ethyl acetate

toluene

反応条件

後処理

1. 1
   洗浄washed with water (3×25 mL)
2. 2
   乾燥The organic layer was dried over sodium sulphate
3. 3
   濃縮concentrated

実験手順

To a solution of 13 (250 mg, 1.010 mmol) in toluene 10 mL was added 3-(trifluoromethyl) picolinaldehyde (177.0 mg, 1.010 mmol). PTSA (384.5 mg, 2.021 mmol) was added to the reaction mixture and 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 (E)-6-methoxy-5-morpholino-2-((3-(trifluoromethyl)pyridin-2-yl)methylene)-2,3-dihydro-1H-inden-1-one 67. The compound 67 was purified through flash chromatography by using 100-200 mesh silica gel. The compound was eluted at 34% ethyl acetate in hexane to afford yellow coloured solid.

出典