Hydrochloric Acid → Styrenesulfonic acid

HRID 484555

반응식

HRID 484555 반응식
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

참가 물질

8

반응물 4

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

생성물 1

HCID 168625Styrenesulfonic acid수율 72%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a5f53cc6049841da99bde5ea89d32326
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05231223

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