تفاعل #90531

ord-9d530a18371d4bc7ad2425b0bc08caa1

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed with water (3×25 mL)
  2. 2
    تجفيفThe organic layer was dried over sodium sulphate
  3. 3
    تركيزconcentrated
  4. 4
    أخرىto get the crude 85 which
  5. 5
    أخرىwas purified through flash chromatography
  6. 6
    غسيلThe compound 85 was eluted at 28% ethyl acetate in hexane

الإجراء التجريبي

To a solution of 13 (100 mg, 04048 mmol) in toluene 10 mL was added 4-(trifluoromethyl)benzaldehyde 84 (70.4 mg, 0.404 mmol). PTSA (153.9 mg, 0.809 mmol) was added to the reaction mass, then stirred at 120° C. for 6 h. The reaction mass was diluted with ethyl acetate and washed with water (3×25 mL). The organic layer was dried over sodium sulphate and concentrated to get the crude 85 which was purified through flash chromatography by using 100-200 mesh silica gel. The compound 85 was eluted at 28% ethyl acetate in hexane to afford yellow coloured solid compound (E)-6-methoxy-5-morpholino-2-(4-(trifluoromethyl)benzylidene)-2,3-dihydro-1H-inden-1-one 85.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09446047B2uspto-grants-2016_09