Water → 4-Oxo-1-iodo-trans-1-octene

HRID 126726

반응식

HRID 126726 반응식
[OH:1][CH:2]([CH2:7][CH2:8][CH2:9][CH3:10])[CH2:3]/[CH:4]=[CH:5]/[I:6].O.O.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].O.S(=O)(=O)(O)O>CCOCC>[I:6]/[CH:5]=[CH:4]/[CH2:3][C:2](=[O:1])[CH2:7][CH2:8][CH2:9][CH3:10]

참가 물질

6

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 108005Sodium dichromate dihydrateHCID 12851278HCID 12851278, 화합물

생성물 1

HCID 128512804-Oxo-1-iodo-trans-1-octene

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of 6.4 g. of 4-hydroxy-1-iodo-trans-1-octene (U.S. Pat. No. 4,061,671, Ex. 4) in 25 ml. of ether, cooled in an ice-bath under argon, is added dropwise over 15 minutes, 25 ml. of a solution prepared by dissolving 100 g. of sodium dichromate dihydrate in 300 ml. of water, followed by 136 g. of sulfuric acid with ice-bath cooling and subsequent dilution to 500 ml. After addition, the mixture is stirred at room temperature for 2 hours and diluted with ether. The ether phase is separated and saved. The aqueous phase is extracted with ether. The ether solutions are combined, washed with saturated sodium chloride solution, 5% sodium thiosulfate solution, twice with saturated sodium chloride solution, dried over magnesium sulfate and taken to dryness, giving the product as an orange oil.

후처리

  1. additionis added dropwise over 15 minutes
  2. customof a solution prepared
  3. dissolutionby dissolving 100 g
  4. additionAfter addition
  5. customThe ether phase is separated
  6. extractionThe aqueous phase is extracted with ether
  7. washwashed with saturated sodium chloride solution, 5% sodium thiosulfate solution, twice with saturated sodium chloride solution
  8. dry with materialdried over magnesium sulfate

출처 및 근거

ORD 기록
ord-9f27ed1469a7497aa4a2f184c9209746
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254036

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