تفاعل #74908

ord-d3a6c63b4a5c415e88d600c12938b6bd

المتفاعلات

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
-20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىremains between -10° and -15° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    workup.ADDITIONthe reaction solution is poured onto ice
  4. 4
    أخرىthe precipitate which has separated out
  5. 5
    ترشيحis filtered off
  6. 6
    غسيلwashed with water
  7. 7
    أخرىThe crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone
  8. 8
    أخرىrises to 126°-128° C.

الإجراء التجريبي

86.0 g (0.51 mole) of 5-chloro-1-indanone are introduced in portions into 540 ml of fuming nitric acid (d=1.54), cooled to -20° C., so that the temperature of the reaction mixture remains between -10° and -15° C. After the addition has ended, the mixture is subsequently stirred for 45 minutes at -15° to -20° C., the reaction solution is poured onto ice and the precipitate which has separated out is filtered off and washed with water. The crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone rises to 126°-128° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04174397uspto-grants-1979_11