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

HRID 1834782
ノート
印刷プレビュー

反応式

HRID 1834782 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5f58dd70e3ba44e080e7a704c696beaa
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04071524

反応ノート

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