تفاعل #2446057
ord-2cc6163a0a734a11a6984c56790720d4
معادلة التفاعل
N-methylpyrrolidone
6-chloro-1H,3H-benzo[de]isochromene-1,3-dione
cystamine hydrochloride
NMP
diisopropylethylamine
→
2,2′-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione)
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةthe mixture is heated
- 2workup.STIRRINGwith stirring at 120° C. for 3 hours
- 3درجة الحرارةAfter cooling
- 4أخرىthe precipitated product is recovered
- 5workup.ADDITIONthe filtered solution is extended by addition of 200 ml of water
- 6أخرىa second precipitate is recovered
- 7غسيلThe precipitates are washed with water
- 8أخرىdried
- 9أخرى11.46 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.