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Bromoacetic Acid → (4-Fluoro-2-nitro-phenylamino)-acetic acid

HRID 1422698
ノート
印刷プレビュー

反応式

HRID 1422698 の反応式
Br[CH2:2][C:3]([OH:5])=[O:4].[F:6][C:7]1[CH:12]=[CH:11][C:10]([NH2:13])=[C:9]([N+:14]([O-:16])=[O:15])[CH:8]=1.[NH4+].[OH-]>C1(C)C(C)=CC=CC=1>[F:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][CH2:2][C:3]([OH:5])=[O:4])=[C:9]([N+:14]([O-:16])=[O:15])[CH:8]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6227Bromoacetic AcidHCID 14923Ammonium HydroxideHCID 677694-Fluoro-2-nitroaniline

生成物 1

HCID 23337266(4-Fluoro-2-nitro-phenylamino)-acetic acid収率 43.5%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
120 °C

実験手順

Bromoacetic acid (5.34 g, 32.0 mmol, 0.5 eq) is added dropwise to 4-fluoro-2-nitro-phenylamine (10.0 g, 64.1 mmol, 1.0 eq) at 120° C. After the addition, the reaction mixture is stirred for 2 hours at 120° C. then xylene (10 mL) is added. The resulting reaction mixture is heated at 130° C. for 1 hour, then it is made alkaline with 25% ammonia aqueous solution. Xylene is removed under reduced pressure and the residue is diluted with water (100 mL). The mixture is filtered at 60° C. and the insoluble residue is extracted twice with 10% ammonia aqueous solution at 60° C. The aqueous layer is acidified with hydrochloric acid to pH 5, the precipitated product is filtered, washed with water and ethanol, dried under vacuum to afford (4-fluoro-2-nitro-phenylamino)-acetic acid as a red solid (2.98 g, 34% yield).

後処理

  1. additionAfter the addition
  2. customThe resulting reaction mixture
  3. temperatureis heated at 130° C. for 1 hour
  4. customXylene is removed under reduced pressure
  5. additionthe residue is diluted with water (100 mL)
  6. filtrationThe mixture is filtered at 60° C.
  7. extractionthe insoluble residue is extracted twice with 10% ammonia aqueous solution at 60° C
  8. filtrationthe precipitated product is filtered
  9. washwashed with water and ethanol
  10. customdried under vacuum

出典と根拠

ORDレコード
ord-b4f8591906ef4686804fc83c50396e05
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08927542B2

反応ノート

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