تفاعل #90562

ord-19b8e5b3de1d45c78f0b4c8371ecb9a4

المذيبات

ظروف التفاعل

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 263, which
  5. 5
    أخرىwas purified through flash chromatography
  6. 6
    غسيلThe compound was eluted at 30% ethyl acetate in hexane

الإجراء التجريبي

To a solution of 13 (0.1 g, 0.40 mmol)), MeOH/H2O (1:1), was added 5-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)nicotinaldehyde 259 (0.132 g, 0.485 mmol) and NaOH (0.032 g, 0.80 mmol). The reaction was stirred at RT for 6 h. The reaction mass was diluted with chloroform and washed with water (3×25 ml). The organic layer was dried over sodium sulphate and concentrated to get the crude 263, which was purified through flash chromatography by using 100-200 mesh silica gel. The compound was eluted at 30% ethyl acetate in hexane to afford yellow coloured solid (E)-2-((5-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)pyridin-3-yl)methylene)-6-methoxy-5-morpholino-2,3-dihydro-1H-inden-1-one 263.

المصدر

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