Ethylene Glycol → HCID 567357, 화합물

HRID 365159노트

반응식

HRID 365159 반응식
[CH:1]12[CH2:8][C:7](=[O:9])[CH:6]1[CH2:5][CH2:4][CH:3]=[CH:2]2.[CH2:10](O)[CH2:11][OH:12].C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)(O)[O-].[Na+]>C1C=CC=CC=1>[O:9]1[CH2:10][CH2:11][O:12][C:7]21[CH2:8][CH:1]1[CH:6]2[CH2:5][CH2:4][CH:3]=[CH:2]1

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 516892Sodium BicarbonateHCID 12507350Bicyclo[4.2.0]oct-2-en-7-one

생성물 1

HCID 567357HCID 567357, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of 6.4 g bicyclo[4.2.0]oct-2-en-7-one (III), (Tetrahedron, 27, 615 (1971)), 18.62 g ethylene glycol, 100 ml benzene, and 25 mg p-toluenesulfonic acid is heated at reflux for 4 hr using a Dean-Stark trap to effect continuous removal of water. The cooled reaction mixture is poured onto 100 ml saturated sodium bicarbonate solution and the resulting mixture is extracted with three 75 ml portions of diethyl ether. The combined organic extract is washed with 100 ml saturated sodium chloride solution and is then dried over sodium sulfate. The solvent is removed under vacuum and the residue is distilled under vacuum to give 7.12 g of spiro[bicyclo[4.2.0]oct-2-ene-7,2'-[1.3]dioxolan] (IV).

후처리

  1. temperatureis heated
  2. temperatureat reflux for 4 hr
  3. customremoval of water
  4. customThe cooled reaction mixture
  5. extractionthe resulting mixture is extracted with three 75 ml portions of diethyl ether
  6. extractionThe combined organic extract
  7. washis washed with 100 ml saturated sodium chloride solution
  8. dry with materialis then dried over sodium sulfate
  9. customThe solvent is removed under vacuum
  10. distillationthe residue is distilled under vacuum

출처 및 근거

ORD 기록
ord-380d3a32eb73444c88dea446be994508
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04608388

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