تفاعل #64265
ord-577526dbb11146de80d79d9d511240ce
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىIn a 250 mL flask equipped with a nitrogen inlet
- 2درجة الحرارةreflux condenser
- 3درجة الحرارةcooled to room temperature
- 4workup.STIRRINGstirred for an additional 16 h
- 5استخلاصthe organics were extracted
- 6تجفيفdried over magnesium sulfate
- 7أخرىthe solvents were removed under reduced pressure
- 8أخرىto yield a yellow powder
- 9أخرىRecrystallization 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.