Water → 3-(Tetradecyloxy)propan-1-ol

HRID 463644

반응식

HRID 463644 반응식
[CH2:1]([OH:5])[CH2:2][CH2:3][OH:4].[CH2:6](Br)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].[OH-].[K+].O>CS(C)=O.O1CCCC1>[CH2:19]([O:4][CH2:3][CH2:2][CH2:1][OH:5])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH3:6]

참가 물질

6

반응물 4

HCID 962WaterHCID 8208Myristyl bromideHCID 104421,3-PropanediolHCID 14797Potassium Hydroxide

생성물 1

HCID 1142393-(Tetradecyloxy)propan-1-ol수율 34.6%

시약·촉매·용매 1

HCID 21830753dimethylsulfoxide THF용매

실험 절차

In 70 ml of a mixture of dimethylsulfoxide-tetrahydrofuran (1:1) are dissolved 12.3 g of trimethylene glycol and 15 g of tetradecyl bromide. To the solution is added 12 g of powdery potassium hydroxide. The mixture is vigorously stirred for one hour at a room temperature, which is refluxed under heating for two hours. The reaction mixture is poured into 400 ml of cold water, which is neutralized and subjected to extraction with ethyl acetate, then washed with water and dried. The resultant is concentrated to dryness, and the residue is dissolved in methanol when hot. Cooling of the solution gives precipitation of crystals, which are removed by filtration. The filtrate is refined by means of chromatography employing silica-gel (eluent:chloroform) to give 5.1 g of the end-product.

후처리

  1. temperaturewhich is refluxed
  2. temperatureunder heating for two hours
  3. extractionsubjected to extraction with ethyl acetate
  4. washwashed with water
  5. customdried
  6. concentrationThe resultant is concentrated to dryness
  7. dissolutionthe residue is dissolved in methanol when hot
  8. temperatureCooling of the solution
  9. customgives
  10. customprecipitation of crystals, which
  11. customare removed by filtration

출처 및 근거

ORD 기록
ord-114af40f277c494d890493369382aa3d
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04544512

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