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Ethanol → Ethyl 4-amino-2,5-difluorobenzoate

HRID 630423
ノート
印刷プレビュー

反応式

HRID 630423 の反応式
[NH2:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:12])[CH:3]=1.[CH2:13](O)[CH3:14].O.C(=O)(O)[O-]>Cl>[NH2:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([O:8][CH2:13][CH3:14])=[O:7])=[C:4]([F:12])[CH:3]=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 4

HCID 702EthanolHCID 769Bicarbonate IonHCID 962WaterHCID 201514774-Amino-2,5-difluorobenzoic acid2 回

生成物 1

HCID 67469350Ethyl 4-amino-2,5-difluorobenzoate収率 92%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

このページの内容参加物実験手順後処理出典と根拠反応ノート

A solution of 4-amino-2,5-difluorobenzoic acid (intermediate 137; 2.7 g; 0.015 mol) in hydrogen chloride 1.25 mL in ethanol (91 mL, 0.113 mol) was stirred for 24 hours at 60° C. The solvent was removed under reduced pressure and the crude obtained was treated with water and solid bicarbonate to obtain a basic pH, after few minutes stirring an extraction with ethyl acetate was done. The organic layer was washed with brine, dried and the solvent was removed under reduced pressure to give the title compound as a white solid (92%), which was used in the next step without further purification.

後処理

  1. customThe solvent was removed under reduced pressure
  2. customthe crude obtained
  3. customto obtain a basic pH
  4. extractionan extraction with ethyl acetate
  5. washThe organic layer was washed with brine
  6. customdried
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-224375bdd5c14bbb9ad8027a3cb5c851
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09315463B2

反応ノート

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