تفاعل #72575

ord-5296c5fb6c684f62a1f52dd25ec74e71

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةmaintaining the temperature between 60 and 70° C
  2. 2
    أخرىis brought to ambient temperature
  3. 3
    workup.WAITAfter 30 minutes
  4. 4
    أخرىthe red solid formed
  5. 5
    ترشيحis filtered off
  6. 6
    غسيلwashed intensively with ice-cold water
  7. 7
    تجفيفit is then dried in vacuo in the presence of P2O5 and at 40° C. overnight

الإجراء التجريبي

Concentrated H2SO4 (20 ml) is heated to 50° C. The compound obtained in Step D (25.24 mmoles) is added slowly in solid form, maintaining the temperature between 60 and 70° C. The reaction mixture is then stirred for one hour at 80° C. The mixture is brought to ambient temperature and then poured onto 200 g of crushed ice. After 30 minutes, the red solid formed is filtered off and washed intensively with ice-cold water; it is then dried in vacuo in the presence of P2O5 and at 40° C. overnight to yield the title product, which is used directly in the next Step.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541412B2uspto-grants-2013_09