반응 #163995

반응 방정식

2-(cyanomethyl)-3-ethyl-1,3-benzothiazol-3-ium iodide

(2Z)-2-[(2E)-3-methoxyprop-2-en-1-ylidene]-1-benzothiophen-3-(2H)-one 1,1-dioxide

CHCl3 MeOH

sodium acetate

→

(2E,3E,5Z)-5-(1,1-dioxido-3-oxo-1-benzothien-2(3H)-ylidene)-2-(3-ethyl-1,3-benzothiazol-2(3H)-ylidene)pent-3-enenitrile

용매

methanol

반응 조건

후처리

1. 1
   기타In a one-necked round bottom 100-mL flask equipped with magnetic stir bar
2. 2
   온도reflux condenser
3. 3
   온도The flask was heated on an oil bath
4. 4
   온도under reflux for an additional 30 min
5. 5
   여과the precipitated solid was filtered
6. 6
   세척washed with methanol
7. 7
   기타dried

실험 절차

In a one-necked round bottom 100-mL flask equipped with magnetic stir bar and reflux condenser were added 2-(cyanomethyl)-3-ethyl-1,3-benzothiazol-3-ium iodide (1.00 g, 3.03 mmol), (2Z)-2-[(2E)-3-methoxyprop-2-en-1-ylidene]-1-benzothiophen-3-(2H)-one 1,1-dioxide (1.00 g, 4.00 mmol) and CHCl3-MeOH mixture (1:1, 20 mL). The flask was heated on an oil bath with stirring until boiling began, and a solution of sodium acetate (320 mg, 4.00 mmol) in 10 mL of methanol was added to the flask. The stirring was continued under reflux for an additional 30 min. The flask was cooled to room temperature and the precipitated solid was filtered, washed with methanol and dried. Green crystals. The yield was 730 mg (57% of theory).

출처