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Water → 1-Vinyl-4-ethyl-2,6,7-trioxabicyclo[2,2,2] octane

HRID 2295528
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HRID 2295528 반응식
Br[CH:2]([C:4]12[O:11][CH2:10][C:7]([CH2:12][CH3:13])([CH2:8][O:9]1)[CH2:6][O:5]2)[CH3:3].CC(C)([O-])C.[K+].O>O1CCCC1>[CH:2]([C:4]12[O:5][CH2:6][C:7]([CH2:12][CH3:13])([CH2:8][O:9]1)[CH2:10][O:11]2)=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 204748331-(1-Bromoethyl)-4-ethyl-2,6,7-trioxabicyclo[2.2.2]octaneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 136431181-Vinyl-4-ethyl-2,6,7-trioxabicyclo[2,2,2] octane수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

25 g (0.1 moles) of the product obtained in step (b) above was added dropwise over about one hour at room temperature to a solution of 11 g (0.1 moles) of potassium t-butoxide in 100 ml of tetrahydrofuran placed in a 250 ml flask. The mixture was heated at reflux temperature for 5 hours and the reaction solution obtained was poured into water. The resulting solution was extracted with ethyl ether and the organic layer was dried over anhydrous magnesium sulfate and concentrated by evaporation of the ether. The residue was distilled under reduced pressure to give 14 g (83%) of the title compound with a boiling point of 68°-72° C./2 mmHg and a specific gravity of 1.216 (Method D).

후처리

  1. customplaced in a 250 ml flask
  2. temperatureThe mixture was heated
  3. temperatureat reflux temperature for 5 hours
  4. customthe reaction solution obtained
  5. extractionThe resulting solution was extracted with ethyl ether
  6. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated by evaporation of the ether
  8. distillationThe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-ecbeaa48e4b5451d9e52edf1263ad5fb
출처 데이터셋
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04425473

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