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

HRID 1601749
ノート
印刷プレビュー

反応式

HRID 1601749 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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 %).

後処理

  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

出典と根拠

ORDレコード
ord-c06eb6fc8bd74f6a804d34be9daa10eb
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05977413

反応ノート

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