反应 #90535

ord-65876cc90a1f43ca8dcca6c2507984b4

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with water (3×25 mL)
  2. 2
    干燥The organic layer was dried over sodium sulphate
  3. 3
    浓缩concentrated
  4. 4
    其他to get the crude 94
  5. 5
    其他was purified through flash chromatography

实验过程

To a solution of 13 (100 mg, 0.404 mmol) in toluene 10 mL was added 3-methyl-1H-pyrazole-5-carbaldehyde 93 (70.8 mg, 0.404 mmol). PTSA (153.8 mg, 0.808 mmol) was added to the reaction mass, then stirred at 120° C. for 6 h, 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 94 and was purified through flash chromatography by using 100-200 mesh silica gel eluting at 2% MeOH in DCM to afford yellow coloured solid compound (E)-6-methoxy-2-((3-methyl-1H-pyrazol-5-yl)methylene)-5-morpholino-2, 3-dihydro-1H-inden-1-one 94.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09446047B2uspto-grants-2016_09