Benzyl mercaptan → 2-Benzylsulfanylmethylacrylic acid

HRID 1830118

반응식

HRID 1830118 반응식
Br[CH2:2][C:3](=[CH2:7])[C:4]([OH:6])=[O:5].[CH2:8]([SH:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[OH-].[Na+]>CO>[CH2:8]([S:15][CH2:2][C:3](=[CH2:7])[C:4]([OH:6])=[O:5])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 7509Benzyl mercaptanHCID 14798Sodium HydroxideHCID 5588842-(Bromomethyl)propenoic acid

생성물 1

HCID 220539822-Benzylsulfanylmethylacrylic acid수율 89%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-Bromomethylacrylic acid (3.00 g, 18.1 mmol) was dissolved in methanol (100 mL), cooled on an ice bath and treated with benzyl mercaptan. Aqueous sodium hydroxide (1N, 39.8 mL) was added dropwise and the reaction mixture was allowed to adjust to room temperature with stirring for 23 hours. Methanol was removed by rotary evaporation at reduced pressure and water (100 mL) was added to the residue, which was then washed with ether. The aqueous layer was cooled on ice and acidified to pH 2.5. The precipitated solid was isolated by filtration and dried to give 2-benzylsulfanylmethyl-acrylic acid (3.346 g, 89%).

후처리

  1. temperaturecooled on an ice bath
  2. customto adjust to room temperature
  3. customMethanol was removed by rotary evaporation at reduced pressure and water (100 mL)
  4. additionwas added to the residue, which
  5. washwas then washed with ether
  6. temperatureThe aqueous layer was cooled on ice
  7. customThe precipitated solid was isolated by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-24a0c52af7d742c592a0060f98d03793
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064123B1

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