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

HRID 339817
ノート
印刷プレビュー

反応式

HRID 339817 の反応式
[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]
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 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 164128103-Amino-3-(2,5-difluorophenyl)propanoic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-480882378fb641c5951efc89f0067bfa
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895547B2

反応ノート

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