تفاعل #1751263

ord-ee6a623d63a74f3484eefa9efffc054f

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture is heated
  2. 2
    workup.STIRRINGwith stirring at 120° C. for 3 hours
  3. 3
    درجة الحرارةAfter cooling
  4. 4
    أخرىthe precipitated product is recovered
  5. 5
    workup.ADDITIONthe filtered solution is extended by addition of 200 ml of water
  6. 6
    أخرىa second precipitate is recovered
  7. 7
    غسيلThe precipitates are washed with water
  8. 8
    أخرىdried
  9. 9
    أخرى11.46 g of white powder are recovered

الإجراء التجريبي

9.30 g of 6-chloro-1H,3H-benzo[de]isochromene-1 ,3-dione and 4.46 g of hydrochlorided cystamine hydrochloride are suspended in 50 ml of N-methylpyrrolidone (NMP). 5.5 g of diisopropylethylamine are added and the mixture is heated with stirring at 120° C. After two hours, 50 ml of NMP are added and the mixture is kept with stirring at 120° C. for 3 hours. After cooling, the precipitated product is recovered and the filtered solution is extended by addition of 200 ml of water, and a second precipitate is recovered. The precipitates are washed with water and dried. 11.46 g of white powder are recovered. The analyses show that the product is in accordance with the expected product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08038731B2uspto-grants-2011_10