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

HRID 47008

반응식

HRID 47008 반응식
[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

참가 물질

4

반응물 2

HCID 85689Hexahydrophthalic anhydrideHCID 1230504-Bromo-2-fluoroaniline

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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°.

후처리

  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°

출처 및 근거

ORD 기록
ord-1d4620b96e2e43209313027423520cda
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04175948

연결된 노트

불러오는 중…