Hydrochloric Acid → 2-Benzyl-3-mercaptopropanoic acid

HRID 248705

反応式

HRID 248705 の反応式
C([S:4][CH2:5][CH:6]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:7]([OH:9])=[O:8])(=O)C.[OH-].[Na+].Cl>CO>[SH:4][CH2:5][CH:6]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:7]([OH:9])=[O:8]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 99917962-[(Acetylthio)methyl]-3-phenylpropionic Acid

生成物 1

HCID 1943272-Benzyl-3-mercaptopropanoic acid収率 52.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

2-Acetylthiomethyl-3-phenylpropionic acid (18.5 g) is mixed with 70% aqueous methanol (100 ml), and the mixture is stirred at room temperature for one hour under nitrogen while maintaining at pH 13.0 with 20% aqueous sodium hydroxide solution, and thereafter the mixture is adjusted to pH 2.0 with 20% hydrochloric acid, and methanol is distilled off under reduced pressure. The residue is purified by a column chromatography using Diaion HP-20 (eluant, water-acetonitrile). The fractions containing the desired compound are collected and acetonitrile is distilled off under reduced pressure. The aqueous solution is extracted with ethyl acetate. The extract is dried over anhydrous magnesium sulfate, and ethyl acetate is distilled off under reduced pressure to give 2-mercaptomethyl-3-phenylpropionic acid (8 g) as a colorless oily substance. IR (film; cm-1): 1700

後処理

  1. distillationis distilled off under reduced pressure
  2. customThe residue is purified by a column chromatography
  3. additionThe fractions containing the desired compound
  4. customare collected
  5. distillationacetonitrile is distilled off under reduced pressure
  6. extractionThe aqueous solution is extracted with ethyl acetate
  7. dry with materialThe extract is dried over anhydrous magnesium sulfate, and ethyl acetate
  8. distillationis distilled off under reduced pressure

出典と根拠

ORDレコード
ord-eec3208194b746639ffacfd617a1244c
出典データセット
uspto-grants-1993_05
特許番号
US05210266

関連ノート

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