Methanethiol → 3-(4-Methoxybenzylmercapto)-2-(methylthio)propanoic acid

HRID 903500

反応式

HRID 903500 の反応式
Br[CH:2]([CH2:6][S:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=1)[C:3]([OH:5])=[O:4].[CH3:17][SH:18].[OH-].[Na+]>C(O)C>[CH3:16][O:15][C:12]1[CH:13]=[CH:14][C:9]([CH2:8][S:7][CH2:6][CH:2]([S:18][CH3:17])[C:3]([OH:5])=[O:4])=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 878MethanethiolHCID 14798Sodium HydroxideHCID 203852902-Bromo-3-(4-methoxybenzylmercapto)propanoic acid

生成物 1

HCID 540570183-(4-Methoxybenzylmercapto)-2-(methylthio)propanoic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-bromo-3-(4-methoxybenzylmercapto) propanoic acid (15 g.), methylmercaptan (3 g.) and sodium hydroxide (4.6 g.) in 95% ethanol (25 ml.) is refluxed for twelve hours. The sodium bromide is filtered off and the filtrate is concentrated to dryness in vacuo. The residue is dissolved in water, acidified with concentrated hydrochloric acid and extracted with ethyl acetate. The organic layer is dried and concentrated to dryness to yield 3-(4-methoxybenzylmercapto)-2-(methylthio)propanoic acid.

後処理

  1. filtrationThe sodium bromide is filtered off
  2. concentrationthe filtrate is concentrated to dryness in vacuo
  3. dissolutionThe residue is dissolved in water
  4. extractionextracted with ethyl acetate
  5. customThe organic layer is dried
  6. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-69fea8a1cdc34979a55d22ad4e70897d
出典データセット
uspto-grants-1980_10
特許番号
US04228077

関連ノート

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