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Diphenyl Ether → HCID 178526468, 화합물

HRID 1394118
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HRID 1394118 반응식
C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.C1(OC2C=CC=CC=2)C=CC=CC=1.C(O[C:44](=[O:64])[CH:45]=[C:46]([NH:54][C:55]1[CH:60]=[CH:59][C:58]([N+:61]([O-:63])=[O:62])=[CH:57][CH:56]=1)[C:47]1[CH:52]=[CH:51][CH:50]=[C:49]([F:53])[CH:48]=1)CCC>>[F:53][C:49]1[CH:48]=[C:47]([C:46]2[CH:45]=[C:44]([OH:64])[C:56]3[C:55](=[CH:60][CH:59]=[C:58]([N+:61]([O-:63])=[O:62])[CH:57]=3)[N:54]=2)[CH:52]=[CH:51][CH:50]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 7583Diphenyl EtherHCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)HCID 69202260HCID 69202260, 화합물

생성물 1

HCID 178526468HCID 178526468, 화합물수율 96%

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온도
250 °C

실험 절차

In a 3 L three-neck flask, equipped with mechanical stirrer, Claisen adapter holding a thermocouple probe and reflux condenser with nitrogen inlet was added 0.75 L of Dowtherm A (a eutectic mixture of 26.5% diphenyl and 73.5% diphenyl oxide) The solvent is then preheated to 250° C. To this was cautiously added in small portions 77.0 grams (0.215 moles) of 3-(4-nitro-phenylamino)-3-(3-fluorophenyl)-acrylic acid butyl ester over the course of 0.25 hours. The mixture was maintained at 250° C. for 1.5 hours and then allowed to cool to 90° C. over the course of 2 hours. The mixture was treated with 1.0 L of hexanes, and allowed to cool to room temperature while stirring overnight. The tan solids were collected by suction filtration and washed with three 0.15 L portions of hexanes. The solids were dried under vacuum at 50° C. overnight to yield 58.63 grams (96.0%) of the title compound.

후처리

  1. customIn a 3 L three-neck flask, equipped with mechanical stirrer
  2. temperaturereflux condenser with nitrogen inlet
  3. customis then preheated to 250° C
  4. temperatureto cool to 90° C. over the course of 2 hours
  5. temperatureto cool to room temperature
  6. filtrationThe tan solids were collected by suction filtration
  7. washwashed with three 0.15 L portions of hexanes
  8. customThe solids were dried under vacuum at 50° C. overnight

출처 및 근거

ORD 기록
ord-c4f32e0e04694167b509fec87bdc8d6f
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07348340B2

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