Ethylene Glycol → 2-[(6-Chloropyrimidin-4-yl)oxy]ethan-1-ol

HRID 2311

반응식

HRID 2311 반응식
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[CH2:9]([OH:12])[CH2:10][OH:11].[H-].[Na+]>O1CCCC1>[Cl:1][C:2]1[N:3]=[CH:4][N:5]=[C:6]([O:11][CH2:10][CH2:9][OH:12])[CH:7]=1

참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 24758Sodium hydrideHCID 709434,6-Dichloropyrimidine

생성물 1

HCID 125648862-[(6-Chloropyrimidin-4-yl)oxy]ethan-1-ol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of 4,6-dichloropyrimidine (5.0 g), ethylene glycol (100 ml) and tetrahydrofuran (100 ml)is added sodium hydride (60% dispersion-type, 1.34 g) under ice-cooling. The mixture is stirred at the same temperature for two hours, and evaporated to remove the solvent. The residue is extracted with ethyl acetate, and the ethyl acetate extract is dried, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1) to give 2-(6-chloropyrimidin-4-yloxy)ethanol (5.67 g) as an oily product.

후처리

  1. temperaturecooling
  2. customevaporated
  3. customto remove the solvent
  4. extractionThe residue is extracted with ethyl acetate
  5. extractionthe ethyl acetate extract
  6. customis dried
  7. concentrationconcentrated under reduced pressure
  8. customThe residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1)

출처 및 근거

ORD 기록
ord-f570953042144533ac7122491f64e455
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728706

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