تفاعل #564948

ord-77680cd18be344df961fd91dc3435a0b

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe mixture was stirred at this temperature for a further hour
  2. 2
    أخرىThe yellow solid was collected
  3. 3
    غسيلwashed with water
  4. 4
    ترشيحThe hot suspension was filtered
  5. 5
    غسيلthe undissolved residue was washed with 200 ml of ether

الإجراء التجريبي

2-Ethoxalylamino-1-nitronaphthalene (11.5 g, 0.04 mol) was dissolved in 80 ml of sulfuric acid (d 1.84) by portionwise addition, with vigorous stirring on an ice-bath. Nitric acid (1.66 ml, 0.04 mol, d 1.52) in 20 ml of sulfuric acid (d 1.84) was added dropwise during 1 h at 0° C., and the mixture was stirred at this temperature for a further hour. The mixture was cautiously poured into 600 ml of ice/water with vigorous stirring. The yellow solid was collected, washed with water, and boiled with 300 ml of ethanol. The hot suspension was filtered and the undissolved residue was washed with 200 ml of ether to yield 7.35 g (55%) of the title compound,

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04889855uspto-grants-1989_12