Hydroquinone → Potassium dobesilate

HRID 587810

反応式

HRID 587810 の反応式
[C:1]1([CH:8]=[CH:7][C:5]([OH:6])=[CH:4][CH:3]=1)[OH:2].CCCCCCC.[S:16](=O)(=[O:19])([OH:18])[OH:17].C(C(CCCC)C([O-])=O)C.[K+:31]>C(OCC)(=O)C>[K+:31].[OH:2][C:1]1[CH:8]=[CH:7][C:5]([OH:6])=[CH:4][C:3]=1[S:16]([O-:19])(=[O:18])=[O:17]

参加物

6

反応物 4

HCID 785HydroquinoneHCID 1118Sulfuric AcidHCID 8900HeptaneHCID 23669619Potassium 2-ethylhexanoate

生成物 1

HCID 23672329Potassium dobesilate収率 96.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
12.5 °C

実験手順

Hydroquinone (20 g, 0.1816 mol) and n-heptane (60 mL) was taken in a round bottom flask, after cooling the flask to about 10-15° C., sulfuric acid (36 N, 17.8 g) was added dropwise at the same temperature and stirring continued further for about 10-15 min. The temperature was slowly raised to 50-60° C. then stirred for 3-8 h. The reaction mass was then cooled to 25-35° C., n-heptane was decanted and ethyl acetate (200 mL) added to dissolve the solid formed. A solution of potassium 2-ethylhexanoate (36.4 g, 0.1996 mol) in ethyl acetate (200 mL) was added slowly. The reaction was further stirred for an hour. The precipitated crude solid was filtered, washed with ethyl acetate to give 40 g of 2,5-dihydroxybenzenesulfonic acid potassium salt.

後処理

  1. temperatureThe temperature was slowly raised to 50-60° C.
  2. stirringthen stirred for 3-8 h
  3. temperatureThe reaction mass was then cooled to 25-35° C.
  4. customn-heptane was decanted
  5. additionethyl acetate (200 mL) added
  6. dissolutionto dissolve the solid
  7. customformed
  8. stirringThe reaction was further stirred for an hour
  9. customThe precipitated crude solid
  10. filtrationwas filtered
  11. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-f2e3b518a908402e83ccb91b631e39bc
出典データセット
uspto-grants-2016_01
特許番号
US09227928B2

関連ノート

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