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

HRID 1058082ノート

反応式

HRID 1058082 の反応式
[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]

参加物

4

反応物 3

HCID 8857Ethyl AcetateHCID 32484DiisopropylanilineHCID 690433-Nitrophthalic acid

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-36faf1f4419641c1b3091703320cfe01
出典データセット
uspto-grants-2003_02
特許番号
US06515129B1

反応ノート

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