Hydrochloric Acid → Styrenesulfonic acid

HRID 484555

反応式

HRID 484555 の反応式
N[C:2]1[C:3]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][CH:5]=[CH:6][CH:7]=1.Cl.N([O-])=O.[Na+].[C:17]([O-])(=O)[CH3:18].[Na+]>[OH-].[Na+].[Pd].CO>[CH2:17]=[CH:18][C:2]1[C:3]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 69262-Aminobenzenesulfonic acidHCID 517045Sodium AcetateHCID 23668193Sodium Nitrite

生成物 1

HCID 168625Styrenesulfonic acid収率 72%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

10.1 g of aniline-2-sulphonic acid (85%) were dissolved in 40 ml of sodium hydroxide solution (6%) and treated with 40 ml of conc. HCl. 12 ml of aqueous NaNO2 solution were added dropwise to the resulting suspension at a temperature of 0° to 5° C. and the mixture was stirred at this temperature for 30 minutes. 50 g of sodium acetate, 300 ml of methanol and 0.5 g of bis(dibenzylideneacetone-2,2'-disulphonic acid disodium salt)palladium(0) were added successively and the mixture was stirred for 3 hours at 20° C. under an ethylene pressure of 20 bar. It was then filtered and evaporated to dryness, and the residue was stirred with ethanol. The mixture was again filtered and evaporated. 7.4 g (72%) of styrene-2-sulphonic acid, Na salt, were obtained.

後処理

  1. stirringthe mixture was stirred for 3 hours at 20° C. under an ethylene pressure of 20 bar
  2. filtrationIt was then filtered
  3. customevaporated to dryness
  4. stirringthe residue was stirred with ethanol
  5. filtrationThe mixture was again filtered
  6. customevaporated

出典と根拠

ORDレコード
ord-a5f53cc6049841da99bde5ea89d32326
出典データセット
uspto-grants-1993_07
特許番号
US05231223

関連ノート

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