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Hydrochloric Acid → Hydroxyphenylacetic acid

HRID 463906
Notes
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Reaction equation

HRID 463906 reaction equation
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([CH:6]=[C:7](Cl)Cl)=[CH:4][CH:3]=1.[OH-:12].[Na+].Cl.C[OH:16]>>[OH:1][C:2]1[CH:11]=[CH:10][C:5]([CH2:6][C:7]([OH:16])=[O:12])=[CH:4][CH:3]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 5324901Phenol, 4-(2,2-dichloroethenyl)-

Product 1

HCID 127Hydroxyphenylacetic acidYield 94.5%

Procedure

In an autoclave were placed 0.5 g of p-hydroxy-β,β-dichlorostyrene ##STR12## 1.0 g of sodium hydroxide and 5 ml of methanol. The mixture was heated at 120°-130° C. for 4 hours. Then the methanol was distilled off. To the residue was added 10 ml of water and the mixture was refluxed for 30 minutes. After completion of the reaction, the reaction mixture was acidified by concentrated hydrochloric acid and was extracted three times with 10 ml of ether. The extract was dried over anhydrous magnesium sulfate and the ether was distilled off. The residue was purified by silica gel column chromatography by using benzene, n-hexane and ethyl acetate (10:10:3) as a developer solvent to afford 0.3 g of p-hydroxyphenylacetic acid ##STR13## Yield 94.5%, m.p. 151°-152° C. NMR (CDCl3, δ, ppm) 3.50 (s, 2H), 4.25 (b.s., 2H), 6.92 (m, 4H)

Workup

  1. temperatureThe mixture was heated at 120°-130° C. for 4 hours
  2. distillationThen the methanol was distilled off
  3. additionTo the residue was added 10 ml of water
  4. temperaturethe mixture was refluxed for 30 minutes
  5. customAfter completion of the reaction
  6. extractionwas extracted three times with 10 ml of ether
  7. dry with materialThe extract was dried over anhydrous magnesium sulfate
  8. distillationthe ether was distilled off
  9. customThe residue was purified by silica gel column chromatography

Sources & evidence

ORD record
ord-0b54db041fb94ea8a71afa1474c46191
Source dataset
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04544766

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes