تفاعل #5727

ord-4b7507acb22e4bf8a1321040f57cb521

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter some time a substance crystallizes out
  2. 2
    غسيلwashed with benzene
  3. 3
    أخرىAfter drying the weight
  4. 4
    أخرىbeing 185° C. with spontaneous decomposition on the Kofler
  5. 5
    درجة الحرارةheating bench
  6. 6
    أخرىit may be recrystallized from 250 ml of benzene with a yield of 80%

الإجراء التجريبي

16.0 g of 2,6-dichlorobenzoylisocyanate are added in small portions to a solution of 11.66 g of p-chloroaniline-acetonitrile in 100 ml of dry benzene with moderate cooling. After some time a substance crystallizes out, which after about 12 hours is drawn off and washed with benzene. After drying the weight is 25.25 g, i.e. 93.7% the melting point being 185° C. with spontaneous decomposition on the Kofler heating bench. Thin-layer chromatography (solvent either ethylacetate or chloroform) shows that the substance is pure, however, if desired, it may be recrystallized from 250 ml of benzene with a yield of 80%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05245071uspto-grants-1993_09