Sulfuric Acid → HCID 14372231、化合物

HRID 1381717ノート

反応式

HRID 1381717 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][C:3]=1[C:11]([OH:13])=[O:12].OS(O)(=O)=O>C(O)(C)C.OS(O)(=O)=O>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([O:10][CH:2]([CH3:7])[CH3:3])=[O:9])[CH:5]=[CH:4][C:3]=1[C:11]([O:13][CH:5]([CH3:6])[CH3:4])=[O:12]

参加物

5

反応物 2

HCID 1118Sulfuric AcidHCID 747852-Chloroterephthalic acid

生成物 1

HCID 14372231HCID 14372231、化合物

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 3776Isopropanol溶媒

実験手順

To 2.0 g of product from Example 1 suspended in 25 ml of isopropyl alcohol was added 0.3 ml of conc. H2SO4 and the reaction mixture heated at reflux for about 18 hours. Conc. H2SO4 (5 drops) was then added and heating continued for an additional 24 hours. The reaction mixture was cooled to room temperature. The solvent was removed and the residue treated with 50 ml of saturated sodium bicarbonate solution and 50 ml of ethyl acetate. The organic phase was dried over sodium sulfate and the solvent removed under nitrogen. Dissolution in pentane followed by removal of the solvent gave the above product.

後処理

  1. temperaturethe reaction mixture heated
  2. temperatureat reflux for about 18 hours
  3. temperatureheating
  4. customThe solvent was removed
  5. additionthe residue treated with 50 ml of saturated sodium bicarbonate solution and 50 ml of ethyl acetate
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. customthe solvent removed under nitrogen
  8. dissolutionDissolution in pentane
  9. customfollowed by removal of the solvent
  10. customgave the above product

出典と根拠

ORDレコード
ord-baea4a33f56042d1beeb86ba3e79f8b5
出典データセット
uspto-grants-1989_02
特許番号
US04803294

反応ノート

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