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Hydrochloric Acid → Ethyl 3-amino-3-(2,5-difluorophenyl)propanoate

HRID 339817
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HRID 339817 반응식
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][CH:6]([C:11]1[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:12]=1[F:18])[CH2:7][C:8](O)=[O:9].Cl>C(O)C>[CH2:1]([O:3][C:8](=[O:9])[CH2:7][CH:6]([NH2:5])[C:11]1[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:12]=1[F:18])[CH3:2]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 164128103-Amino-3-(2,5-difluorophenyl)propanoic acid

생성물 1

HCID 43312570Ethyl 3-amino-3-(2,5-difluorophenyl)propanoate

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

Acetyl chloride (4 ml) was added dropwise at room temperature to a round-bottom flask containing ethanol (50 ml). 3-Amino-3-(2,5-difluorophenyl)propionic acid (2.94 g) was added to the ethanolic hydrochloric acid solution thus prepared, and the mixture was stirred at 50° C. for three hours. Subsequently, the mixture was concentrated under reduced pressure, and the residue was admixed with 1N sodium hydroxide solution (100 ml) and extracted immediately with dichloromethane (3×50 ml). The combined organic phases were dried (Na2SO4), filtered and concentrated. The product (3.2 g) was used without further purification.

후처리

  1. customthus prepared
  2. concentrationSubsequently, the mixture was concentrated under reduced pressure
  3. extractionextracted immediately with dichloromethane (3×50 ml)
  4. dry with materialThe combined organic phases were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe product (3.2 g) was used without further purification

출처 및 근거

ORD 기록
ord-480882378fb641c5951efc89f0067bfa
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08895547B2

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