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Pentaerythritol → 2,2-Dibutyl-1,3,2-dioxastanninane

HRID 1265232
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HRID 1265232 반응식
[CH2:1]([Sn:5](=[O:10])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[OH:11][CH2:12][C:13](CO)(CO)[CH2:14]O>C1(C)C=CC=CC=1>[CH2:1]([Sn:5]1([CH2:6][CH2:7][CH2:8][CH3:9])[O:11][CH2:12][CH2:13][CH2:14][O:10]1)[CH2:2][CH2:3][CH3:4]
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참가 물질

4

반응물 2

HCID 8285PentaerythritolHCID 61221Dibutyltin oxide

생성물 1

HCID 166927232,2-Dibutyl-1,3,2-dioxastanninane수율 87.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

49.78 g (0.2 mol) of dibutyltin oxide and 13.615 g (0.1 mol) of pentaerythritol were introduced into a 1000 ml reaction vessel equipped with a Dean-Stark device, and the atmosphere in the reaction vessel was replaced by argon. 500 ml of toluene was added, and the mixture was dehydrated by azeotropic distillation at 130° C. and stirred for 26.5 hours during which it became an uniform solution. After left and cooled to room temperature, the precipitated white solids were filtered. The white solids were heated and dissolved in 300 ml of toluene, and cooled gradually to room temperature, and the precipitated white solids were filtered. The resulting white solids were dried at 60° C. for 5 hours in vaccuo to give 4,4′-spirobi[1,1-dibutylstanna-2,6-dioxacyclohexane, 52.3 g (87.5% yield).

후처리

  1. customequipped with a Dean-Stark device
  2. distillationthe mixture was dehydrated by azeotropic distillation at 130° C.
  3. waitAfter left
  4. filtrationthe precipitated white solids were filtered
  5. temperatureThe white solids were heated
  6. dissolutiondissolved in 300 ml of toluene
  7. temperaturecooled gradually to room temperature
  8. filtrationthe precipitated white solids were filtered
  9. customThe resulting white solids were dried at 60° C. for 5 hours in vaccuo

출처 및 근거

ORD 기록
ord-5195132024384b2cb4527de427f4ef1c
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06545112B2

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