Hydrochloric Acid → 3-(Acetylthio)-2-[(acetylthio)methyl]propanoic acid

HRID 1252826

反応式

HRID 1252826 の反応式
[C:1]([OH:4])(=[S:3])[CH3:2].Br[CH2:6][CH:7]([CH2:11]Br)[C:8]([OH:10])=[O:9].Cl>[OH-].[K+]>[C:1]([S:3][CH2:6][CH:7]([CH2:11][S:3][C:1](=[O:4])[CH3:2])[C:8]([OH:10])=[O:9])(=[O:4])[CH3:2]

参加物

5

実験手順

A solution of 3.36 g (40 mmoles) of thioacetic acid in 40 ml of N-potassium hydroxide is added dropwise to a solution of 2-bromomethyl-3-bromopropanoic acid in 1.0N potassium hydroxide (20 ml). The mixture is stirred at room temperature overnight, acidified with concentrated hydrochloric acid and extracted with ethyl acetate. The organic layer is dried and concentrated in vacuo. The residue is converted into a dicyclohexylammonium salt (m.p. 116°-118°) and the salt converted back into the free acid, 2-(acetylthiomethyl)-3-(acetylthio)propanoic acid, by distribution between ethyl acetate and 10% potassium bisulfate.

後処理

  1. extractionextracted with ethyl acetate
  2. customThe organic layer is dried
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f0094c45a9b94187bcd71483166700ed
出典データセット
uspto-grants-1988_05
特許番号
US04745124

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