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1-(3-Hydroxy-4-nitro-2,5,6-trifluorophenoxy)-3-benzyloxy-4-nitrobenzene → 3-(3-Hydroxy-4-amino-2,5,6-trifluorophenoxy)-6-aminophenol

HRID 430057
ノート
印刷プレビュー

反応式

HRID 430057 の反応式
[OH:1][C:2]1[C:3]([F:31])=[C:4]([C:23]([F:30])=[C:24]([F:29])[C:25]=1[N+:26]([O-])=O)[O:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-])=O)=[C:8]([O:15]CC2C=CC=CC=2)[CH:7]=1.[H][H]>O1CCCC1.C(OCC)(=O)C.[Pd]>[OH:1][C:2]1[C:3]([F:31])=[C:4]([C:23]([F:30])=[C:24]([F:29])[C:25]=1[NH2:26])[O:5][C:6]1[CH:7]=[C:8]([OH:15])[C:9]([NH2:12])=[CH:10][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 183538411-(3-Hydroxy-4-nitro-2,5,6-trifluorophenoxy)-3-benzyloxy-4-nitrobenzeneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 183538363-(3-Hydroxy-4-amino-2,5,6-trifluorophenoxy)-6-aminophenol

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

43.6 g of 1-(3-hydroxy-4-nitro-2,5,6-trifluorophenoxy)-3-benzyloxy-4-nitrobenzene prepared as described in Example 13 (0.1 mol) are dissolved in 400 ml of a mixture of tetrahydrofuran and ethyl acetate (volume ratio 1:1), and 4.4 g of Pd/C (palladium/carbon) are added to the solution. The mixture is then hydrogenated at room temperature in an autoclave with vigorous stirring using hydrogen at a pressure of 1 bar; after 3 days, the reaction is terminated. The yellow solution is evaporated to half in a rotary evaporator an left to stand at room temperature overnight, during which the reaction product precipitates in crystalline form. The reaction product is then separated off and dried for 48 hours under nitrogen at, 40° C./10 mbar in a vacuum drying cabinet.

後処理

  1. additionare added to the solution
  2. customis then hydrogenated at room temperature in an autoclave
  3. customthe reaction is terminated
  4. customThe yellow solution is evaporated to half in a rotary evaporator
  5. waitan left
  6. waitto stand at room temperature overnight, during which
  7. customthe reaction product precipitates in crystalline form
  8. customThe reaction product is then separated off
  9. customdried for 48 hours under nitrogen at, 40° C./10 mbar in a vacuum
  10. customdrying cabinet

出典と根拠

ORDレコード
ord-f31172241dc04831885b7123486b289f
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06320081B1

反応ノート

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