Sulfuric Acid → Glyceryl methacrylate

HRID 722666

反応式

HRID 722666 の反応式
[CH2:1]([O:5][C:6](=[O:10])[C:7]([CH3:9])=[CH2:8])[CH:2]1[O:4][CH2:3]1.C[O:12]C1C=CC(O)=CC=1.S(=O)(=O)(O)O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O>[C:6]([O:5][CH2:1][CH:2]([CH2:3][OH:12])[OH:4])(=[O:10])[C:7]([CH3:9])=[CH2:8]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 7837Glycidyl methacrylateHCID 90154-MethoxyphenolHCID 24436Sodium Sulfate

生成物 1

HCID 65442Glyceryl methacrylate収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into a two phase mixture of 86 g (0.6 mol) of comercial glycidylmethacrylate containing 200 ppm of MEHQ and 500 ml of water is added 2 ml of concentrated sulfuric acid at ambient temperature. After stirring approximately 18 hours, the mixture appeared as a clear homogenous solution. To the resultant solution is added sufficient sodium sulfate to cause separation of an oil. The 2 phase mixture is extracted sequentially with 5 portions of 150 ml each of chloroform and the combined chloroform extracts are dried over solid sodium sulfate. After filtering the solid sodium sulfate, the solvent is removed by evaporation to give 77 g (80%) of glycerol mono-methacrylate as a clear colorless oil. The monomer can be used without further purification or can be further purified by chromatography to separate trace amounts of glycerol di-methacrylate.

後処理

  1. customseparation of an oil
  2. extractionThe 2 phase mixture is extracted sequentially with 5 portions of 150 ml each of chloroform
  3. dry with materialthe combined chloroform extracts are dried over solid sodium sulfate
  4. filtrationAfter filtering the solid sodium sulfate
  5. customthe solvent is removed by evaporation

出典と根拠

ORDレコード
ord-3c76a2f843a94fe98f011185866b09ce
出典データセット
uspto-grants-2006_11
特許番号
US07138457B2

関連ノート

読み込み中…