2,6-Dimethylaniline → 1,3(2H,4H)-Isoquinolinedione, 2-(2,6-dimethylphenyl)-

HRID 2301920노트

반응식

HRID 2301920 반응식
[C:1]1(=[O:12])[O:7][C:5](=O)[C:4]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:3]2[CH2:2]1.[CH3:13][C:14]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:15]=1[NH2:16]>C(OCC)(=O)C>[CH3:13][C:14]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:15]=1[N:16]1[C:5](=[O:7])[C:4]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:3]2[CH2:2][C:1]1=[O:12]

참가 물질

4

반응물 2

HCID 68962,6-DimethylanilineHCID 12801Homophthalic anhydride

생성물 1

HCID 1827511,3(2H,4H)-Isoquinolinedione, 2-(2,6-dimethylphenyl)-수율 68%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

0.67 g (4.13 mmol) of homophthalic anhydride and 0.4 g (3.30 mmol) of 2,6-dimethylaniline were mixed, and melted at a temperature of 200° C. for 1 hour. The reactant was dissolved in ethyl acetate, washed with aqueous NaHCO3 solution, with water and then with saturated aqueous sodium chloride, dried over anhydrous MgSO4, and subjected to filtration with a folded filter paper. The filtrate was concentrated and evaporated to dryness. The residue was recrystallized by using a mixture of CH2Cl2 and hexane, to obtain 0.565 g (yield 68%) of the specified substance as light yellow granulated crystals. It showed the following physical properties and analyzed values.

후처리

  1. washwashed with aqueous NaHCO3 solution, with water
  2. dry with materialwith saturated aqueous sodium chloride, dried over anhydrous MgSO4
  3. filtrationsubjected to filtration with a folded filter paper
  4. concentrationThe filtrate was concentrated
  5. customevaporated to dryness
  6. customThe residue was recrystallized
  7. additiona mixture of CH2Cl2 and hexane
  8. customto obtain 0.565 g (yield 68%) of the specified substance as light yellow granulated crystals

출처 및 근거

ORD 기록
ord-552f155c24d8450bbf5f748cf90a8017
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06429212B1

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