تفاعل #790929

ord-29f55b879e0e43c59ca51901c5dfd064

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe mixture is filtered in order
  2. 2
    أخرىto remove a small quantity of starting material
  3. 3
    workup.ADDITIONtreated with 10 g of vegetable charcoal
  4. 4
    workup.STIRRINGAfter stirring for a few minutes at ambient temperature
  5. 5
    أخرىremoval of the vegetable charcoal
  6. 6
    ترشيحby filtration
  7. 7
    workup.WAITthe solution is left
  8. 8
    أخرىthe expected product which has crystallized
  9. 9
    ترشيحis then filtered off
  10. 10
    أخرىAfter recrystallization from ethanol
  11. 11
    أخرىdrying in vacuo

الإجراء التجريبي

0.3 mol (19.8 g) of 85% by weight potassium hydroxide pellets is dissolved in 210 ml of glycerol, and 0.25 mol (41.75 g) of 3,4-methylenedioxynitrobenzene is then added, with stirring. After heating for one and a half hours in the region of 110° C., the reaction medium is poured into 1.5 liters of iced water. The mixture is filtered in order to remove a small quantity of starting material. The filtrate is acidified to pH=4 with hydrochloric acid and then treated with 10 g of vegetable charcoal. After stirring for a few minutes at ambient temperature and removal of the vegetable charcoal by filtration, the solution is left to stand overnight at 0° C. and the expected product which has crystallized is then filtered off. After recrystallization from ethanol and drying in vacuo, the product melts at 148° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04985042uspto-grants-1991_01