Hydrochloric Acid → 2-Benzyl-3-mercaptopropanoic acid

HRID 248705

반응식

HRID 248705 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 1943272-Benzyl-3-mercaptopropanoic acid수율 52.5%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-eec3208194b746639ffacfd617a1244c
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210266

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