Hydroquinone → Potassium dobesilate

HRID 587812

反応式

HRID 587812 の反応式
[C:1]1([CH:8]=[CH:7][C:5]([OH:6])=[CH:4][CH:3]=1)[OH:2].ClCCl.[S:12](=O)(=[O:15])([OH:14])[OH:13].C(C(CCCC)C([O-])=O)C.[K+:27]>C(OCC)(=O)C>[K+:27].[OH:2][C:1]1[CH:8]=[CH:7][C:5]([OH:6])=[CH:4][C:3]=1[S:12]([O-:15])(=[O:14])=[O:13]

参加物

6

反応物 4

HCID 785HydroquinoneHCID 1118Sulfuric AcidHCID 6344DichloromethaneHCID 23669619Potassium 2-ethylhexanoate

生成物 1

HCID 23672329Potassium dobesilate収率 77.9%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

反応条件

温度
12.5 °C

実験手順

Hydroquinone (10 g, 0.09 mol) and dichloromethane (30 mL), was taken in a round bottom flask, after cooling the flask to about 10-15° C., sulfuric acid (36 N, 8.9 g) was added dropwise at the same temperature and stirring continued further for about 10-15 min. Temperature was slowly raised to 30-40° C. then stirred for 1-2 h. The reaction mass was then cooled to 25-35° C. and ethyl acetate (100 mL) added to dissolve the solid formed. A solution of potassium 2-ethylhexanoate (18.2 g, 0.099 mol) in ethyl acetate (100 mL) was added slowly. The reaction was further stirred for an hour. The precipitated crude solid was filtered, washed with ethyl acetate to give 16 g of 2,5-dihydroxybenzenesulfonic acid potassium salt.

後処理

  1. temperatureTemperature was slowly raised to 30-40° C.
  2. stirringthen stirred for 1-2 h
  3. temperatureThe reaction mass was then cooled to 25-35° C.
  4. dissolutionto dissolve the solid
  5. customformed
  6. stirringThe reaction was further stirred for an hour
  7. customThe precipitated crude solid
  8. filtrationwas filtered
  9. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-06ae9ecef4334649a355952e273299a2
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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