تفاعل #163995

ord-d80d9f75d2f64180ae500e87393d67c8

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىIn a one-necked round bottom 100-mL flask equipped with magnetic stir bar
  2. 2
    درجة الحرارةreflux condenser
  3. 3
    درجة الحرارةThe flask was heated on an oil bath
  4. 4
    درجة الحرارةunder reflux for an additional 30 min
  5. 5
    ترشيحthe precipitated solid was filtered
  6. 6
    غسيلwashed with methanol
  7. 7
    أخرىdried

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08835632B2uspto-grants-2014_09