Hydrochloric Acid → Methyl alpha-methylthio-alpha-(m-benzoylphenyl)propionate

HRID 1277782ノート

反応式

HRID 1277782 の反応式
[CH3:1][S:2][C:3]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15](OC)([O:22]C)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5].COCCOC.O.Cl>C(Cl)Cl>[CH3:1][S:2][C:3]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15](=[O:22])[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 80711,2-DimethoxyethaneHCID 12819452Methyl alpha-methylthio-alpha-(m-(alpha,alpha-dimethoxybenzyl)phenyl)propionate

生成物 1

HCID 13020172Methyl alpha-methylthio-alpha-(m-benzoylphenyl)propionate収率 102.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 978 mg of methyl α-methylthio-α-[m-(α,α-dimethoxybenzyl)phenyl]propionate were added 2 ml of 1,2-dimethoxyethane and 0.5 ml of water, and 0.2 ml of conc. hydrochloric acid was further added. The mixture was stirred at room temperature for 15 hours. The reaction solution was diluted with 50 ml of methylene chloride, and dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and the filtrate was concentrated under reduced pressure to afford 874 mg of methyl α-methylthio-α-(m-benzoylphenyl)propionate. The product was found to be substantially pure by its NMR and GLC.

後処理

  1. additionwas further added
  2. dry with materialdried over anhydrous sodium sulfate
  3. customThe drying agent was separated by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-cada97a3b7674a799a1ef6838417858e
出典データセット
uspto-grants-1981_07
特許番号
US04278802

反応ノート

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