Benzyl mercaptan → 2-Benzylsulfanylmethylacrylic acid

HRID 1830118

反応式

HRID 1830118 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 220539822-Benzylsulfanylmethylacrylic acid収率 89%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-24a0c52af7d742c592a0060f98d03793
出典データセット
uspto-grants-2006_06
特許番号
US07064123B1

関連ノート

読み込み中…