Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ruthenium | HCID 23950 | — |
| Reactant | Tetrakis(dimethylsulfoxide)dichlororuthenium (II) | HCID 150194 | — |
| Reactant | HCID 88050071 | HCID 88050071 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 131724488 | HCID 131724488 | — |
Reaction Steps
2.83 g of (1R,2R)-N-(2-diphenylphosphanylbenzyl)-N′-[2-diphenylphosphanyl-5-(4-vinylbenzyloxy)benzyl]cyclohexan-1,2-diamine (3.5 mmol, 9.4% stabiliser) are refluxed for 1 hour under protective gas with 3.36 g of dichlorotetrakis(dimethyl sulfoxide)ruthenium(II) (7 mmol) in 200 ml of absolute toluene. During the reaction, 120 mg of a yellowish solid precipitate out, which can be identified as a ruthenium-stabiliser complex. Once the reaction solution has been filtered, the solvent is removed in a rotary evaporator and the product separated by column chromatography on silica gel (isohexane/ethyl acetate 2:1). In order to isolate the product, the chromatographic fractions should not be evaporated to dryness, but instead combined with isohexane once the eluent has largely been removed. As a result, the product precipitates as a yellow/orange powder at a yield of 1.86 g (55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06759559B2 |
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| Source dataset | uspto-grants-2004_07 |
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| ORD ID | ord-487fefd2e16b4002bed9481299488e7c |
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| Source note | uspto-grants-2004_07 |
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