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

HRID 15716

反応式

HRID 15716 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-08ae92f127f94ec6a8ff8f48fe108716
出典データセット
uspto-grants-2010_06
特許番号
US07732622B2

関連ノート

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