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Hydrogen Bromide → 3'-Amino-5'-fluoro-2'-hydroxy-biphenyl-3-carboxylic acid hydrobromide

HRID 384347
ノート
印刷プレビュー

反応式

HRID 384347 の反応式
[BrH:1].Cl.[NH2:3][C:4]1[C:5]([OH:20])=[C:6]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([OH:19])=[O:18])[CH:12]=2)[CH:7]=[C:8]([F:10])[CH:9]=1>C(OCC)(=O)C>[BrH:1].[NH2:3][C:4]1[C:5]([OH:20])=[C:6]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([OH:19])=[O:18])[CH:12]=2)[CH:7]=[C:8]([F:10])[CH:9]=1
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 260Hydrogen BromideHCID 574838163'-Amino-5'-fluoro-2'-hydroxy-biphenyl-3-carboxylic acid hydrochloride

生成物 1

HCID 574838233'-Amino-5'-fluoro-2'-hydroxy-biphenyl-3-carboxylic acid hydrobromide収率 54.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

20 mL of hydrobromic acid was added dropwise to 3′-amino-5′-fluoro-2′-hydroxy-biphenyl-3-carboxylic acid 2f (500 mg, 1.92 mmol) obtained from Step 5 of Example 2 to form white precipitates. The reaction solution was heated to reflux overnight, and then it became clear. The colour of the reaction solution finally was brown. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was concentrated under reduced pressure to obtain a brown solid which was dissolved in 20 mL of ethyl acetate. The mixture was stirred for 20 minutes and filtered to obtain the title compound 3′-amino-5′-fluoro-2′-hydroxy-biphenyl-3-carboxylic acid hydrobromide 26a (344 mg, yield 54.8%) as a grey solid.

後処理

  1. customto form white precipitates
  2. temperatureThe reaction solution was heated
  3. temperatureto reflux overnight
  4. concentrationThe mixture was concentrated under reduced pressure
  5. customto obtain a brown solid which
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-6608643e5213464796720169af8a2175
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367710B2

反応ノート

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