HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Sulfide → 3,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Sulfide | HCID 402 | — |
| Reactant | Sodium Sulfide | HCID 14804 | — |
| Reactant | (3-Chloropropyl)triethoxysilane | HCID 78771 | — |
| Reactant | Sulfur | HCID 5362487 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy- | HCID 92506 | — |
Reaction Steps
A mixture of 129 l of ethanol and 129 l of 3-chloropropyltriethoxysilane is placed in the reactor of comparison example 1. 13.85 kg of sulfur in the form of granules is metered in. 35.6 kg of virtually anhydrous sodium sulfide is then added. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction. The reaction mixture is kept for a further 1.5 hours at 82-83° C. and then cooled. The reaction mixture is worked up as in comparison example 1. An almost water-white product is obtained. HPLC analysis confirms in this case too the presence of a polysulfane mixture with a mean chain length of 2, though the mixture has a high monosulfane content.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06465672B2 |
| Source dataset | uspto-grants-2002_10 |
| ORD ID | ord-ea86db37e155412f93250386da05fa5a |
| Source note | uspto-grants-2002_10 |