반응 #47838

ord-e3b1b261e3074333bea20c1dd6c7cfe8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at 0° C
  2. 2
    workup.STIRRINGto be stirred for 15 hrs
  3. 3
    세척The resulting mixture was washed with saturated saline
  4. 4
    추출extracted with dichloromethane
  5. 5
    기타The organic layer was separated
  6. 6
    건조dried over anhydrous MgSO4
  7. 7
    농축concentrated under a reduced pressure
  8. 8
    기타The resulting residue was purified by flash chromatography

실험 절차

1-Amino-6-methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (50 mg, 0.16 mmol) prepared in Example 20 was dissolved in dichloromethane (10 mL), and propionyl chloride (150.38 mg, 0.14 mL, 1.62 mmol) and triethylamine (180.12 mg, 0.25 mL, 1.78 mmol) were added thereto in order at 0° C. The mixture was stirred for 24 hrs at RT, and an excess amount of propionyl chloride (2 mL) was further added thereto to be stirred for 15 hrs. The resulting mixture was washed with saturated saline and extracted with dichloromethane. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 29 mg of the titled compound (yield: 50%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745439B2uspto-grants-2010_06