Hexahydrophthalic anhydride → 2-(4-Bromo-2-fluorophenyl)hexahydro-1H-isoindole-1,3(2H)-dione

HRID 47008

反応式

HRID 47008 の反応式
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([F:9])[CH:3]=1.[CH:10]12[C:19](=O)[O:18][C:16](=[O:17])[CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15]2>C(O)(=O)C>[Br:1][C:2]1[CH:8]=[CH:7][C:5]([N:6]2[C:16](=[O:17])[CH:11]3[CH:10]([CH2:15][CH2:14][CH2:13][CH2:12]3)[C:19]2=[O:18])=[C:4]([F:9])[CH:3]=1

参加物

4

反応物 2

HCID 85689Hexahydrophthalic anhydrideHCID 1230504-Bromo-2-fluoroaniline

生成物 1

HCID 129065652-(4-Bromo-2-fluorophenyl)hexahydro-1H-isoindole-1,3(2H)-dione

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

11.4 Parts of 4-bromo-2-fluoroaniline were added to a solution of 10 parts of cyclohexane-1,2-dicarboxylic anhydride in 100 parts of glacial acetic acid and the mixture was stirred for 2 hours. The mixture was refluxed for 20 hours and then poured onto 200 parts of ice. The resulting purple crystals were filtered and recrystallized from 70 parts of methanol at -40° to yield 7.6 parts of lavender crystals of 2-(4-bromo-2-fluorophenyl)-3a,4,5,6,7,7a-hexahydro-1H-isoindole-1,3(2H)-dione melting at 90°-92°.

後処理

  1. temperatureThe mixture was refluxed for 20 hours
  2. additionpoured onto 200 parts of ice
  3. filtrationThe resulting purple crystals were filtered
  4. customrecrystallized from 70 parts of methanol at -40°

出典と根拠

ORDレコード
ord-1d4620b96e2e43209313027423520cda
出典データセット
uspto-grants-1979_11
特許番号
US04175948

関連ノート

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