Bis(dimethylamino)dimethylsilane → 3,3,6,6,9,9-Hexamethyl-1,2,4,5-tetraoxa-3-silacyclononane

HRID 971831

반응식

HRID 971831 반응식
[CH3:1][C:2]([O:11][OH:12])([CH2:4][CH2:5][C:6]([CH3:10])([O:8][OH:9])[CH3:7])[CH3:3].CN([Si:16](N(C)C)([CH3:18])[CH3:17])C>CCOCC>[CH3:17][Si:16]1([CH3:18])[O:12][O:11][C:2]([CH3:1])([CH3:3])[CH2:4][CH2:5][C:6]([CH3:10])([CH3:7])[O:8][O:9]1

참가 물질

4

반응물 2

HCID 77384Bis(dimethylamino)dimethylsilaneHCID 5204702,5-Dimethylhexane 2,5-dihydroperoxide

생성물 1

HCID 213119193,3,6,6,9,9-Hexamethyl-1,2,4,5-tetraoxa-3-silacyclononane수율 97.8%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
16 °C

실험 절차

Into a 250 ml flask equipped with a magnetic stirring bar, addition funnel and calcium sulfate drying tube is placed a solution of 10.84g (0.06 mole, 98.66% pure) of 2,5-dimethyl-2,5-dihydroperoxyhexane in 120 ml of anhydrous ether. The solution is cooled to 16° C. and a solution of 8.77g (0.06 mole) of bis(dimethylamino) dimethylsilane in 30 ml of anhydrous ether is added slowly dropwise. The reaction temperature is maintained between 15° and 20° by use of an ice bath and by adjusting the rate of addition. After the addition is complete, the solution is stirred at room temperature for one hour. The solution is filtered to remove a small amount of suspended solid. The solvent is removed by distillation yielding 13.75g of 3,3,6,6,9,9-hexamethyl-1,2,4,5-tetraoxa-3-silacyclononane (theoretical yield 14.05g, 97.9%; A.O. analysis 13.32%, theoretical 13.67%, 97.4% pure). The infrared spectrum of the reaction product of this example is identical to the spectrum of material produced in Example 1.

후처리

  1. customInto a 250 ml flask equipped with a magnetic stirring bar, addition funnel and calcium sulfate drying tube
  2. temperatureThe reaction temperature is maintained between 15° and 20° by use of an ice bath
  3. additionthe rate of addition
  4. additionAfter the addition
  5. filtrationThe solution is filtered
  6. customto remove a small amount of suspended solid
  7. customThe solvent is removed by distillation

출처 및 근거

ORD 기록
ord-ce90ff2921424486a3dd2f34914212c2
출처 데이터셋
uspto-grants-1979_07
특허 번호
US04161485

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