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

HRID 991955
ノート
印刷プレビュー

反応式

HRID 991955 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14804Sodium Sulfide4 回HCID 78771(3-Chloropropyl)triethoxysilaneHCID 5362487Sulfur

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bdddaa50fe714a9893bdfe247ed5b474
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06465672B2

反応ノート

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