تفاعل #64265

ord-577526dbb11146de80d79d9d511240ce

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىIn a 250 mL flask equipped with a nitrogen inlet
  2. 2
    درجة الحرارةreflux condenser
  3. 3
    درجة الحرارةcooled to room temperature
  4. 4
    workup.STIRRINGstirred for an additional 16 h
  5. 5
    استخلاصthe organics were extracted
  6. 6
    تجفيفdried over magnesium sulfate
  7. 7
    أخرىthe solvents were removed under reduced pressure
  8. 8
    أخرىto yield a yellow powder
  9. 9
    أخرىRecrystallization from acetone

الإجراء التجريبي

In a 250 mL flask equipped with a nitrogen inlet, overhead stirring assembly, and reflux condenser were placed 3-nitrobenzoyl chloride (28 g, 0.15 mol), bromobenzene (130 g, 0.83 mol), and aluminum chloride (22 g, 0.16 mol). The mixture was heated for 3 h at 100° C., then cooled to room temperature and stirred for an additional 16 h. The mixture was poured into 1 L of acidic (HCl) ice water, and the organics were extracted using methylene chloride, dried over magnesium sulfate, and the solvents were removed under reduced pressure to yield a yellow powder. Recrystallization from acetone afforded 42.1 g (90% yield) of white crystals: m.p. 104°-105° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05412066uspto-grants-1995_05