Potassium Hydroxide → 3-(o-Hydroxymethylphenylthio)-4-hydroxybenzoic acid

HRID 2418496노트

반응식

HRID 2418496 반응식
[SH:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][OH:5].I[C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][C:19]=1[OH:20])[C:14]([OH:16])=[O:15].[OH-].[K+]>O.[Cu]>[OH:5][CH2:4][C:3]1[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=1[S:1][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][C:19]=1[OH:20])[C:14]([OH:16])=[O:15]

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 1382782-MercaptobenzenemethanolHCID 4494734-Hydroxy-3-iodobenzoic acid (2IPCOOH)

생성물 1

HCID 202039813-(o-Hydroxymethylphenylthio)-4-hydroxybenzoic acid

시약·촉매·용매 2

HCID 23978Copper촉매HCID 962Water용매2회

실험 절차

A mixture of 25 g o-mercaptobenzyl alcohol (0.18 mole), 39.6 g 3-iodo-4-hydroxy benzoic acid (0.15 mole), 11.43 g copper powder (0.18 mole), 70 ml 40% aqueous potassium hydroxide solution (0.5 mole) and 300 ml water was placed under nitrogen atmosphere and stirred under reflux for 18 hours. After cooling the mixture was diluted with 400 ml of water and extracted twice with 100 ml of ethyl acetate to remove neutral products. The aqueous fraction was filtered and the filtrate acidified with conc. HCl to afford the title compound as an oil which solidified and was filtered. There was obtained 32.8 g solid.

후처리

  1. temperatureunder reflux for 18 hours
  2. temperatureAfter cooling the mixture
  3. extractionextracted twice with 100 ml of ethyl acetate
  4. customto remove neutral products
  5. filtrationThe aqueous fraction was filtered

출처 및 근거

ORD 기록
ord-1deed9c350d74db3a5f0cd7fe6a2e4b0
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04472586

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