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2,4,6-Trifluoroaniline → 2-(2,4,6-Trifluorophenyl)hexahydro-1H-isoindole-1,3(2H)-dione

HRID 1288041
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HRID 1288041 반응식
[F:1][C:2]1[CH:8]=[C:7]([F:9])[CH:6]=[C:5]([F:10])[C:3]=1[NH2:4].[CH:11]12[C:20](=O)[O:19][C:17](=[O:18])[CH:12]1[CH2:13][CH2:14][CH2:15][CH2:16]2>C(O)(=O)C>[F:1][C:2]1[CH:8]=[C:7]([F:9])[CH:6]=[C:5]([F:10])[C:3]=1[N:4]1[C:17](=[O:18])[CH:12]2[CH:11]([CH2:16][CH2:15][CH2:14][CH2:13]2)[C:20]1=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 677652,4,6-TrifluoroanilineHCID 85689Hexahydrophthalic anhydride

생성물 1

HCID 203847012-(2,4,6-Trifluorophenyl)hexahydro-1H-isoindole-1,3(2H)-dione

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

9.54 Parts of 2,4,6-trifluoroaniline were added to a solution of 10 parts of cyclohexane-1,2-dicarboxylic anhydride in 100 parts of glacial acetic acid. The mixture was refluxed for 20 hours and the resulting mixture was poured into 200 parts of ice. The resulting crystals were filtered, dried and recrystallized twice from 70 parts of methanol at -40° C to yield 8.3 parts of white crystals of 2-(2,4,6-trifluorophenyl)-3a,4,5,6,7,7a-hexahydro-1H-isoindole-1,3(2H)-dione melting at 129°-131° C.

후처리

  1. temperatureThe mixture was refluxed for 20 hours
  2. additionthe resulting mixture was poured into 200 parts of ice
  3. filtrationThe resulting crystals were filtered
  4. customdried
  5. customrecrystallized twice from 70 parts of methanol at -40° C

출처 및 근거

ORD 기록
ord-ac7d8bcc216440ed99a565f73ad5dd93
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03987057

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