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

HRID 1058083ノート

反応式

HRID 1058083 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

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 ethanol

出典と根拠

ORDレコード
ord-ecfac2b319f64097a7b6f1ea70497d0d
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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