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Hydrochloric Acid → Methyl 2-chloro-3-hydroxycarbonyl-4-methylsulfonylbenzoate

HRID 1276119
ノート
印刷プレビュー

反応式

HRID 1276119 の反応式
O.P([O-])([O-])(O)=O.[Na+].[Na+].OO.[Cl-].[Na+].[Cl:13][C:14]1[C:23]([CH:24]=[O:25])=[C:22]([S:26]([CH3:29])(=[O:28])=[O:27])[CH:21]=[CH:20][C:15]=1[C:16]([O:18][CH3:19])=[O:17].Cl.S([O-])(O)=[O:32].[Na+]>O.C(#N)C>[Cl:13][C:14]1[C:23]([C:24]([OH:32])=[O:25])=[C:22]([S:26]([CH3:29])(=[O:28])=[O:27])[CH:21]=[CH:20][C:15]=1[C:16]([O:18][CH3:19])=[O:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 5234Sodium ChlorideHCID 61488Phosphoric acid, disodium salt, hydrateHCID 18517410Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoateHCID 23665763Sodium Bisulfite

生成物 1

HCID 18517418
Methyl 2-chloro-3-hydroxycarbonyl-4-methylsulfonylbenzoate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
5 °C

実験手順

At 5° C., 13.8 g (0.11 mol) of sodium hydrogen phosphate monohydrate in 170 ml of water, 49.3 g (0.43 mol) of a 30% strength solution of hydrogen peroxide and 66.2 g (0.59 mol) of an 80% strength aqueous sodium chloride solution were added successively to a solution of 115.3 g (0.42 mol) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate and 2000 ml of acetonitrile. The reaction solution was subsequently stirred at 5° C. for 1 hour and then at room temperature for 12 hours. The pH was then adjusted to 1 using 10% strength hydrochloric acid, and 1500 ml of aqueous 40% strength sodium hydrogen sulfite solution were added. The mixture was stirred at room temperature for 1 hour and the aqueous phase was extracted three times with ethyl acetate. The combined organic phases were washed with sodium hydrogen sulfite solution and dried. The solvent was distilled off, yielding 102.0 g of methyl 2-chloro-3-hydroxycarbonyl-4-methylsulfonylbenzoate.

後処理

  1. waitat room temperature for 12 hours
  2. additionwere added
  3. stirringThe mixture was stirred at room temperature for 1 hour
  4. extractionthe aqueous phase was extracted three times with ethyl acetate
  5. washThe combined organic phases were washed with sodium hydrogen sulfite solution
  6. customdried
  7. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-0f2f3b3e043b4135bb196d3103e24d0e
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06165944

反応ノート

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