Potassium Hydroxide → HCID 13102419、化合物

HRID 648222ノート

反応式

HRID 648222 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 13102419HCID 13102419、化合物収率 16.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-34a7a48af6a24a33a7a87794fd28379d
出典データセット
uspto-grants-1983_10
特許番号
US04411908

反応ノート

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