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

HRID 2301918노트

반응식

HRID 2301918 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([OH:15])=O)[C:7](=[CH:11][CH:12]=1)[C:8]([OH:10])=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(OCC)(=O)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:8](=[O:10])[C:7]2=[CH:11][CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=[C:6]2[C:13]1=[O:15])([CH3:28])[CH3:27]

참가 물질

4

반응물 2

HCID 32484DiisopropylanilineHCID 691211,2-Benzenedicarboxylic acid, 4-nitro-

생성물 1

HCID 137848352-(2,6-Diisopropylphenyl)-5-nitroisoindoline-1,3-dione수율 50%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

0.386 g of anhydride obtained by dehydrating 4-nitrophthalic acid (including 20% of 3-nitrophthalic acid) at a temperature of about 190° 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 ethanol, to obtain 0.352 g (yield 50%) 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 ethanol

출처 및 근거

ORD 기록
ord-7c2be0f63c7c4eedb9ada7c5916cd642
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06429212B1

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