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Sodium Sulfide → 3,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy-

HRID 991955
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HRID 991955 반응식
[S-2:1].[Na+].[Na+].[S].Cl[CH2:6][CH2:7][CH2:8][Si:9]([O:16][CH2:17][CH3:18])([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12]>C(O)C>[CH2:11]([O:10][Si:9]([CH2:8][CH2:7][CH2:6][S:1][S:1][CH2:6][CH2:7][CH2:8][Si:9]([O:16][CH2:17][CH3:18])([O:10][CH2:11][CH3:12])[O:13][CH2:14][CH3:15])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])[CH3:12]
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참가 물질

5

반응물 3

HCID 14804Sodium Sulfide4회HCID 78771(3-Chloropropyl)triethoxysilaneHCID 5362487Sulfur

생성물 1

HCID 925063,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy-

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

17.8 kg of virtually anhydrous sodium sulfide are mixed with 190 l of ethanol and added to an enameled 500 l capacity reactor. This is followed by the addition through a fine nozzle of 13.85 kg of sulfur in molten form. The mixture is heated to 50° C. and 190 l of 3-chloropropyltriethoxysilane are metered in within 10 minutes. On account of the exothermic reaction the temperature of the reactor contents rises to 74° C. A further 4.45 kg of virtually anhydrous sodium sulfide are added at this temperature. Three further portions of sodium sulfide are added at 5 minute intervals (i.e. each 5 minutes), the temperature of the reactor contents rising to 82° C. After completion of the sodium sulfide addition the reaction mixture is kept for 1.5 hours at 82-83° C. and the sodium chloride that has precipitated is separated after cooling the mixture. A yellow product is obtained after evaporating the reaction mixture in vacuo and renewed fine filtration. HPLC analysis confirms the presence of a product with a mean polysulfane chain length of 2.

후처리

  1. additionadded to an enameled 500 l capacity reactor
  2. customare metered in within 10 minutes
  3. customOn account of the exothermic reaction the temperature of the reactor contents
  4. customrises to 74° C
  5. customrising to 82° C
  6. customthe sodium chloride that has precipitated
  7. customis separated
  8. temperatureafter cooling the mixture
  9. customA yellow product is obtained
  10. customafter evaporating the reaction mixture in vacuo
  11. filtrationfiltration

출처 및 근거

ORD 기록
ord-bdddaa50fe714a9893bdfe247ed5b474
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06465672B2

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