Potassium Hydroxide → HCID 13102419, 화합물

HRID 648222노트

반응식

HRID 648222 반응식
[OH:1][CH2:2][C:3]1([CH3:12])[CH2:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[O:4]1.[OH-].[K+].[Mn]([O-])(=O)(=O)=[O:16].[K+].S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+]>O>[CH3:12][C:3]1([C:2]([OH:16])=[O:1])[CH2:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[O:4]1

참가 물질

6

반응물 4

HCID 14797Potassium HydroxideHCID 516875Potassium PermanganateHCID 656671Sodium PyrosulfiteHCID 20482667(2-Methyl-2,3-dihydro-1-benzofuran-2-yl)methanol

생성물 1

HCID 13102419HCID 13102419, 화합물수율 16.9%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

The 2-hydroxymethyl-2-methyl-2,3-dihydrobenzofuran (16.4 g) and potassium hydroxide (5.2 g) in water (150 ml) were mixed and cooled to 5°. Potassium permanganate (20 g) was added portionwise over 45 minutes to the stirred mixture maintained below 12°. After the addition was complete stirring was continued for 1 hour and the mixture was then diluted with water. Sodium metabisulphite was added to destroy the precipitated MnO2 followed by an excess of sodium carbonate. The basic aqueous phase was washed with methylene chloride and then acidified with 2 N hydrochloric acid. Extraction with methylene chloride followed by washing, drying and evaporation of the extracts gave the carboxylic acid (3.0 g); I.R. νmax 1720 cm-1.

후처리

  1. temperaturecooled to 5°
  2. temperaturemaintained below 12°
  3. additionAfter the addition
  4. customto destroy the precipitated MnO2
  5. washThe basic aqueous phase was washed with methylene chloride
  6. extractionExtraction with methylene chloride
  7. washby washing
  8. customdrying
  9. customevaporation of the extracts

출처 및 근거

ORD 기록
ord-34a7a48af6a24a33a7a87794fd28379d
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04411908

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