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

HRID 630423
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HRID 630423 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 769Bicarbonate IonHCID 962WaterHCID 201514774-Amino-2,5-difluorobenzoic acid2회

생성물 1

HCID 67469350Ethyl 4-amino-2,5-difluorobenzoate수율 92%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

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.

후처리

  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

출처 및 근거

ORD 기록
ord-224375bdd5c14bbb9ad8027a3cb5c851
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315463B2

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