تفاعل #67941

ord-470fd18e4c004da9bf043eb5c0be01eb

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىMost of the solvent was evaporated
  2. 2
    ترشيحthe precipitate was filtered
  3. 3
    غسيلwashed with Et2O
  4. 4
    أخرىDrying under hv

الإجراء التجريبي

The aforementioned mixture of amides 14a/14b (500 mg, 1.43 mmol) was suspended in glacial acetic acid (8 mL) and heated to 90° C. for 7 h. Most of the solvent was evaporated, and the yellow residue was suspended in Et2O. After being vigorously stirred for 20 min, the precipitate was filtered and washed with Et2O. Drying under hv gave 404 mg (85%) of 15 as a beige solid. Data of 15: Rf 0.80 (hexane/EtOAc 1:5). 1H NMR (300 MHz, DMSOd6): δ 3.76 (s, 3H), 4.14 (s, 3H), 4.34 (s, 3H), 7.14-7.17 (m, 1H), 7.48-7.55 (m, 3H), 8.25 (s, 1H). MS (ESI): m/z (rel intensity) 331 (98).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524899B2uspto-grants-2013_09