Water → Ethyl [4-(4,9-diethoxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate

HRID 15716

반응식

HRID 15716 반응식
[CH2:1]([O:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([O:14][CH2:15][CH3:16])=[C:6]2[C:17]([O:19][C:20](=O)[C:5]=12)=[O:18])[CH3:2].[NH2:22][C:23]1[CH:28]=[CH:27][C:26]([CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])=[CH:25][CH:24]=1.O>C(O)(=O)C>[CH2:33]([O:32][C:30](=[O:31])[CH2:29][C:26]1[CH:25]=[CH:24][C:23]([N:22]2[C:20](=[O:19])[C:5]3[C:4]([O:3][CH2:1][CH3:2])=[C:13]4[CH:12]=[CH:11][CH:10]=[CH:9][C:8]4=[C:7]([O:14][CH2:15][CH3:16])[C:6]=3[C:17]2=[O:18])=[CH:28][CH:27]=1)[CH3:34]

참가 물질

5

반응물 3

HCID 962WaterHCID 225219p-Aminophenylacetic acid ethyl esterHCID 207619774,9-Bis(ethyloxy)naphtho[2,3-c]furan-1,3-dione

생성물 1

HCID 20761976Ethyl [4-(4,9-diethoxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate

시약·촉매·용매 1

HCID 176Acetic Acid용매

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%.

후처리

  1. filtrationThe white solid was filtered
  2. washwashed with water
  3. dissolutiondissolved in dichloromethane (800 ml)
  4. washThe solution was washed with water, brine
  5. dry with materialdried (MgSO4)
  6. customthe solvent evaporated under vacuum

출처 및 근거

ORD 기록
ord-08ae92f127f94ec6a8ff8f48fe108716
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732622B2

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