Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | HCID 23106070 | HCID 23106070 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 23106072 | HCID 23106072 | — |
Reaction Steps
20.0 ml (152 mmol) of diethylamine are used as initial charge in 1,2-dichloroethane in an inertized three-necked flask with dropping funnel, reflux condenser with hose coupling at its upper end, a tap with hose coupling and a Teflon stirrer bar, in a countercurrent of argon. 10.4 g (29.7 mmol) of 1,6-bis(chlorotrisulphanyl)hexane in 50 ml of 1,2-dichloroethane are then slowly added dropwise, with stirring. The reaction mixture is stirred at room temperature for 4 hours. The resultant salt is filtered off, and the organic phase is washed three times with water and dried over sodium sulphate. After removal of the solvent on a rotary evaporator and drying in the vacuum generated by a rotary-vane pump, 1,6-bis(diethylaminotrisulphanyl)hexane precipitates in the form of a yellow oil. The crude yield is 5.32 g (82%). Elemental analysis was carried out on the crude product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07319124B2 |
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| Source dataset | uspto-grants-2008_01 |
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| ORD ID | ord-4eb204a75d884ca58c15243e35901cc0 |
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| Source note | uspto-grants-2008_01 |
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