Sodium Hydroxide → 68281-27-6

HRID 434522노트

반응식

HRID 434522 반응식
[OH:1][CH2:2][C:3]1([CH3:13])[O:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][CH2:4]1.[OH:14]C1(C)COC2C=CC=CC=2OC1.[OH-].[Na+].[Mn]([O-])(=O)(=O)=O.[K+]>O>[CH3:13][C:3]1([C:2]([OH:14])=[O:1])[O:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][CH2:4]1

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 3778286HCID 3778286, 화합물HCID 126375283-Methyl-3,4-dihydro-2H-1,5-benzodioxepin-3-ol

생성물 1

HCID 1263753668281-27-6

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture (23.7 g) of 2-hydroxymethyl-2-methyl-1,4-benzodioxan and 3-hydroxy-3-methyl-2H-1,5-benzodioxepine (~3:1 ratio; prepared according to the method of A. Salimbeni, E. Manghisi, J. Heterocyclic Chem., 17, 489, 1980) was stirred with 1 N aqueous sodium hydroxide solution (135 ml) and cooled to 0°-10°. A solution of potassium permanganate (42 g) in water (165 ml) was added slowly so that the temperature was maintained below 10°. After 48 hours at room temperature the mixture was filtered and the filtrate acidified with 1 M aqueous sulphuric acid and extracted with methylene chloride. The extracts were washed with aqueous sodium bicarbonate solution and the aqueous layer was acidified with sulphuric acid. Extraction with methylene chloride followed by washing, drying and evaporation of the extracts gave the carboxylic acid (11.5 g); m.p. 125°-129.5°.

후처리

  1. customprepared
  2. temperaturecooled to 0°-10°
  3. temperaturewas maintained below 10°
  4. filtrationAfter 48 hours at room temperature the mixture was filtered
  5. extractionextracted with methylene chloride
  6. washThe extracts were washed with aqueous sodium bicarbonate solution
  7. extractionExtraction with methylene chloride
  8. washby washing
  9. customdrying
  10. customevaporation of the extracts

출처 및 근거

ORD 기록
ord-3d16da0dc31f47b6a489f20ce23e880c
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04397860

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