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Hydrochloric Acid → Hydroxyphenylacetic acid

HRID 463906
ノート
印刷プレビュー

反応式

HRID 463906 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

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

生成物 1

HCID 127Hydroxyphenylacetic acid収率 94.5%

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-0b54db041fb94ea8a71afa1474c46191
出典データセット
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04544766

反応ノート

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