Ethyl Acetate → 2-(2,6-Diisopropylphenyl)-5-nitroisoindoline-1,3-dione

HRID 2301917노트

반응식

HRID 2301917 반응식
[N+:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:6]([C:7]([OH:9])=O)[C:5]=1C(O)=O)([O-:3])=[O:2].[CH:16]([C:19]1[CH:25]=[CH:24][CH:23]=[C:22]([CH:26]([CH3:28])[CH3:27])[C:20]=1[NH2:21])([CH3:18])[CH3:17].[C:29](OCC)(=[O:31])C>>[CH:26]([C:22]1[CH:23]=[CH:24][CH:25]=[C:19]([CH:16]([CH3:18])[CH3:17])[C:20]=1[N:21]1[C:7](=[O:9])[C:6]2=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:12][CH:11]=[C:10]2[C:29]1=[O:31])([CH3:28])[CH3:27]

참가 물질

4

반응물 3

HCID 8857Ethyl AcetateHCID 32484DiisopropylanilineHCID 690433-Nitrophthalic acid

생성물 1

HCID 137848352-(2,6-Diisopropylphenyl)-5-nitroisoindoline-1,3-dione수율 45%

실험 절차

0.386 g of anhydride obtained by dehydrating 3-nitrophthalic acid at a temperature of about 220° C., and 0.354 g of 2,6-diisopropylaniline were mixed, and reacted at a temperature of 180° C. for 4 hours. After the reaction was finished, the reaction mixture was dissolved in ethyl acetate, dried over anhydrous magnesium sulfate and subjected to filtration. The filtrate was concentrated and dried and solidified. Then, it was recrystallized by using a mixture of hexane and ethyl acetate, to obtain 0.320 g (yield 45%) of the specified compound.

후처리

  1. additionwere mixed
  2. customreacted at a temperature of 180° C. for 4 hours
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationsubjected to filtration
  5. concentrationThe filtrate was concentrated
  6. customdried
  7. customThen, it was recrystallized
  8. additiona mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-a2abe7bc554f46cdaa6fbd50b1870023
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06429212B1

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