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2,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane → 2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane

HRID 1601749
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HRID 1601749 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:11]([C:20]2[CH:25]=[CH:24][C:23]([OH:26])=[C:22]([N+:27]([O-])=O)[CH:21]=2)([C:16]([F:19])([F:18])[F:17])[C:12]([F:15])([F:14])[F:13])[CH:7]=[CH:8][C:9]=1[OH:10])([O-])=O>CO>[NH2:27][C:22]1[CH:21]=[C:20]([C:11]([C:6]2[CH:7]=[CH:8][C:9]([OH:10])=[C:4]([NH2:1])[CH:5]=2)([C:12]([F:13])([F:14])[F:15])[C:16]([F:17])([F:18])[F:19])[CH:25]=[CH:24][C:23]=1[OH:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 111336832,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane

생성물 1

HCID 6326032,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

400.0 g of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane and 1200 cc of methanol were put into a 2000-cc four-neck flask equipped with a thermometer, a Dimroth condenser and a stirrer, and stirred therein, to which was added 9.0 g (dry weight) of E196R/W5%Pd. This was heated and kept at 60 to 65° C. with stirring, to which was dropwise added 313.2 g of an aqueous solution of 60% hydrazine monohydrate over a period of 4 hours. After the aqueous hydrazine solution was added, the mixture was stirred for further 30 minutes, and then gradually cooled to room temperature. After the catalyst was removed through filtration, the reaction mixture was concentrated to obtain a crude product of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane. The crude yield was 336.8 g (98%). The purity in liquid chromatography was 97.9% (area %).

후처리

  1. customequipped with a thermometer
  2. additionto which was added
  3. dry with material9.0 g (dry weight) of E196R/W5%Pd
  4. temperatureThis was heated
  5. customkept at 60 to 65° C.
  6. stirringwith stirring, to which
  7. customof 4 hours
  8. additionAfter the aqueous hydrazine solution was added
  9. stirringthe mixture was stirred for further 30 minutes
  10. customAfter the catalyst was removed through filtration
  11. concentrationthe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-c06eb6fc8bd74f6a804d34be9daa10eb
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05977413

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