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Phosgene → 2,5-Bis(2,2,2-trifluoroethoxy)phenyl isocyanate

HRID 2412334
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HRID 2412334 반응식
[C:1](Cl)(Cl)=[O:2].[F:5][C:6]([F:23])([F:22])[CH2:7][O:8][C:9]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][C:18]([F:21])([F:20])[F:19])=[CH:12][C:10]=1[NH2:11]>C1(C)C=CC=CC=1>[F:5][C:6]([F:22])([F:23])[CH2:7][O:8][C:9]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][C:18]([F:21])([F:19])[F:20])=[CH:12][C:10]=1[N:11]=[C:1]=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 133704342,5-Bis(trifluoroethoxy)aniline

생성물 1

HCID 133704362,5-Bis(2,2,2-trifluoroethoxy)phenyl isocyanate

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a cooled (15°-20° C.) solution of 67.6 g. (0.684 mole) of phosgene in 250 ml. of toluene is added dropwise over one hour a solution of 49.5 g. (0.171 mole) of 2,5-bis-(2,2,2-trifluoroethoxy)aniline in 350 ml. of toluene. After addition is complete, stirring is continued for 30 minutes, then the mixture is heated to its reflux temperature and maintained at reflux for 30 minutes. The solution is evaporated to provide a liquid residue which gradually crystallizes. The solid is recrystallized from heptane to provide 2,5-bis(2,2,2-trifluoroethoxy)phenyl isocyanate as a white solid, m.p. 50°-52° C.

후처리

  1. temperatureTo a cooled (15°-20° C.) solution of 67.6 g
  2. additionAfter addition
  3. temperaturethe mixture is heated to its
  4. temperaturereflux temperature
  5. temperaturemaintained
  6. temperatureat reflux for 30 minutes
  7. customThe solution is evaporated
  8. customto provide a liquid residue which
  9. customgradually crystallizes
  10. customThe solid is recrystallized from heptane

출처 및 근거

ORD 기록
ord-75d59ab1fb9741a2aec2b42cc7cfaba8
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04491584

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