Water → MS-1254

HRID 595094

反応式

HRID 595094 の反応式
C[O-].[Na+].[CH3:4][O:5][C:6](=[O:9])[CH2:7][SH:8].Cl[CH2:11][C:12](=[O:14])[CH3:13].O>CO>[CH3:4][O:5][C:6](=[O:9])[CH2:7][S:8][CH2:11][C:12](=[O:14])[CH3:13]

参加物

6

反応物 4

HCID 962WaterHCID 6571ChloroacetoneHCID 16907Methyl ThioglycolateHCID 10942334Sodium Methoxide

生成物 1

HCID 3761561MS-1254

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a mixture of a 5.4 M methanolic solution of sodium methylate (185 mL, 1.00 mol) in 500 mL methanol is added mercapto-acetic acid methyl ester (97.0 g, 912 mmol) at RT. After stirring for 20 minutes at RT chloro acetone (80 mL, 1.0 mmol) is added carefully. After complete addition the reaction mixture is heated at reflux for 20 minutes. The reaction mixture is added to water and extracted with diethyl ether. The organic layer is washed with brine, dried over Na2SO4 and the solvent is evaporated under reduced pressure. The crude reaction product is distilled under reduced pressure (75° C.-90° C., 0.3 mbar) yielding the desired product as colorless liquid. Yield: 61.5 g. (M+H)+=163

後処理

  1. additionis added carefully
  2. additionAfter complete addition the reaction mixture
  3. temperatureis heated
  4. temperatureat reflux for 20 minutes
  5. extractionextracted with diethyl ether
  6. washThe organic layer is washed with brine
  7. dry with materialdried over Na2SO4
  8. customthe solvent is evaporated under reduced pressure
  9. customThe crude reaction product
  10. distillationis distilled under reduced pressure (75° C.-90° C., 0.3 mbar)

出典と根拠

ORDレコード
ord-476cc25d823746b4ae7c75845e272c55
出典データセット
uspto-grants-2016_01
特許番号
US09243000B2

関連ノート

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