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Benzene → Dimethyl Phthalate

HRID 720800
ノート
印刷プレビュー

反応式

HRID 720800 の反応式
[C:1]1(=[O:11])[O:6][C:4](=[O:5])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.S(=O)(=O)(O)O.Cl.S([O:23][CH3:24])(OC)(=O)=O.[CH:25]1C=CC=CC=1>CO>[C:4]([O:23][CH3:24])(=[O:5])[C:3]1[C:2](=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:1]([O:6][CH3:25])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 6497Dimethyl SulfateHCID 6811Phthalic Anhydride

生成物 1

HCID 8554Dimethyl Phthalate

試薬・触媒・溶媒 1

HCID 887Methanol
溶媒

実験手順

Accordingly the present invention provides a method of producing dimethyl phthalate, which comprises treating phthalic anhydride with methanol, adding a catalyst, such as sulphuric acid, hydrochloric acid or mixture thereof and a promoter, such as, dimethyl sulphate; refluxing the resultant mixture at a temperature in the range of 60 to 100 degree Celsius, for a time period in the range of 6 to 12 hours, in the presence of benzene; separating the distillate into two layers; removing the aqueous layer and recycling the benzene layer, recovering unreacted methanol by distillation; neutralizing the residue with caustic soda followed by extraction with benzene; distilling the extract under vacuum to obtain benzene; continuing the distillation process at a temperature in the range of 145 to 146 degree Celsius under 10 mm of mercury to obtain dimethyl phthalate.

後処理

  1. additionadding a catalyst
  2. customin the range of 6 to 12 hours
  3. customseparating the distillate into two layers
  4. customremoving the aqueous layer
  5. customrecovering unreacted methanol
  6. distillationby distillation
  7. extractionfollowed by extraction with benzene
  8. distillationdistilling the
  9. extractionextract under vacuum
  10. customto obtain benzene
  11. customin the range of 145 to 146 degree Celsius

出典と根拠

ORDレコード
ord-40f26d0f734b43f48e3a301f9b0addd1
出典データセット
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07135588B2

反応ノート

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