반응 #43994

ord-08ae92f127f94ec6a8ff8f48fe108716

반응 방정식

CCOc1c2c(c(OCC)c3ccccc13)C(=O)OC2=O
1,4-Diethoxy-2,3-naphthalenedicarboxylic anhydride
CCOC(=O)Cc1ccc(N)cc1
ethyl (4-aminophenyl)acetate
O
water
CCOC(=O)Cc1ccc(N2C(=O)c3c(c(OCC)c4ccccc4c3OCC)C2=O)cc1
ethyl[4-(4,9-diethoxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The white solid was filtered
  2. 2
    세척washed with water
  3. 3
    workup.DISSOLUTIONdissolved in dichloromethane (800 ml)
  4. 4
    세척The solution was washed with water, brine
  5. 5
    건조dried (MgSO4)
  6. 6
    기타the solvent evaporated under vacuum

실험 절차

1,4-Diethoxy-2,3-naphthalenedicarboxylic anhydride (23.3 g, 81.5 mmol) and ethyl (4-aminophenyl)acetate (14.8 g, 82 mmol) were refluxed under nitrogen in acetic acid (160 ml) overnight. The mixture was cooled to room temperature and poured into water (1 L). The white solid was filtered, washed with water and dissolved in dichloromethane (800 ml). The solution was washed with water, brine and dried (MgSO4) and the solvent evaporated under vacuum to give ethyl[4-(4,9-diethoxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate as an off-white solid, 33 g, 96%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732622B2uspto-grants-2010_06