Vinyltrichlorosilane → Vinyltris(furfuryloxy)silane

HRID 1981368

반응식

HRID 1981368 반응식
[CH2:1]([OH:7])[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1.[Na].[CH:9]([Si:11](Cl)(Cl)Cl)=[CH2:10]>C1(C)C=CC=CC=1>[CH:9]([Si:11]([O:7][CH2:1][C:2]1[O:6][CH:5]=[CH:4][CH:3]=1)([O:7][CH2:1][C:2]1[O:6][CH:5]=[CH:4][CH:3]=1)[O:7][CH2:1][C:2]1[O:6][CH:5]=[CH:4][CH:3]=1)=[CH2:10]

참가 물질

5

반응물 3

HCID 6413VinyltrichlorosilaneHCID 7361Furfuryl Alcohol2회HCID 5360545Sodium2회

생성물 1

HCID 20262148Vinyltris(furfuryloxy)silane

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
100 °C

실험 절차

To a solution of 86.5 ml. furfuryl alcohol in 200 ml. toluene was slowly added 23 g. sodium metal. An additional 10 ml. furfuryl alcohol was added and the solution was heated to 100° C. with stirring to convert all the sodium. The solution was cooled to ice temperature and 43.5 ml. vinyltrichlorosilane dissolved in 50 ml. toluene was slowly added. After the addition was complete, the mixture was heated at 95° C. for 0.5 hr. The colloidal sodium chloride by-product was extracted with water. The organic phase was filtered and the toluene removed by vacuum evaporation. The residue was distilled at 2 mmHg and the product recovered at 182°-184° C.

후처리

  1. temperatureThe solution was cooled to ice temperature and 43.5 ml
  2. additionAfter the addition
  3. temperaturethe mixture was heated at 95° C. for 0.5 hr
  4. extractionThe colloidal sodium chloride by-product was extracted with water
  5. filtrationThe organic phase was filtered
  6. customthe toluene removed by vacuum evaporation
  7. distillationThe residue was distilled at 2 mmHg
  8. customthe product recovered at 182°-184° C.

출처 및 근거

ORD 기록
ord-9350b9942400482a94c2f8b9b9aaf1fd
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04514536

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