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http://hdl.handle.net/2445/186109
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DC Field | Value | Language |
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dc.contributor.author | Kennington, Stuart C. D. | - |
dc.contributor.author | Romea, Pedro | - |
dc.contributor.author | Urpí Tubella, Fèlix | - |
dc.date.accessioned | 2022-05-30T16:33:17Z | - |
dc.date.available | 2023-01-31T06:10:27Z | - |
dc.date.issued | 2022-01-31 | - |
dc.identifier.issn | 0078-6209 | - |
dc.identifier.uri | http://hdl.handle.net/2445/186109 | - |
dc.description.abstract | A. [(R)-DTBM-SEGPHOS]NiCl2 (1). An oven--dried single-necked 25 mL round-bottomed flask (14/23 joint), equipped with a 1.5-cm Teflon-coated magnetic stir bar, is charged with (R)-DTBM-SEGPHOS (1.00 g, 0.85 mmol, 1 equiv) (Note 2) and NiCl2 (110 mg, 0.85 mmol, 1 equiv) (Note 3), and acetonitrile (15 mL) (Note 4). A reflux condenser (14/23 joint) with a rubber septum is attached to the round-bottomed flask, and the system is purged for 5 min with N2, after which a N2-filled balloon is used to seal the system. The mixture is then heated at reflux in an oil bath for 16 h. A Number 3 Glass filter funnel connected with a vacuum adaptor to a single-necked 500 mL round-bottomed flask (29/32 joint) is charged with Celite® (25 g) (Note 5). The Celite® is wetted with acetonitrile (70 mL) (Note 4) and allowed to settle. Whilst the reaction mixture is still warm, the contents are poured over the Celite®. Once absorbed, the Celite® is carefully washed (Note 6) with acetonitrile (300 mL) (Note 4) until the color completely passes to the round-bottomed flask. The filtrate is concentrated on a rotary evaporator (30 °C, 12 mmHg). The resulting solid is dissolved in dichloromethane (20 mL) (Note 7) and transferred to a vial (20 mL). The solution is concentrated on a rotary evaporator (30 °C, 12 mmHg) and the resulting solid is broken up with a spatula and dried on a high vacuum line (0.1 mmHg) for 4 h giving the title compound 1 (1.10 g, 0.84 mmol, 99%) (Note 8) as a fine dark green-black powder. | - |
dc.format.extent | 14 p. | - |
dc.format.mimetype | application/pdf | - |
dc.language.iso | eng | - |
dc.publisher | John Wiley & Sons | - |
dc.relation.isformatof | Versió postprint del document publicat a: https://doi.org/10.15227/orgsyn.099.0001 | - |
dc.relation.ispartof | Organic Syntheses, 2022, vol. 99, p. 1-14 | - |
dc.relation.uri | https://doi.org/10.15227/orgsyn.099.0001 | - |
dc.rights | (c) John Wiley & Sons, 2022 | - |
dc.source | Articles publicats en revistes (Química Inorgànica i Orgànica) | - |
dc.subject.classification | Química heterocíclica | - |
dc.subject.classification | Síntesi orgànica | - |
dc.subject.classification | Níquel | - |
dc.subject.other | Heterocyclic chemistry | - |
dc.subject.other | Organic synthesis | - |
dc.subject.other | Nickel | - |
dc.title | Synthesis of [(R)-DTBM-SEGPHOS]NiCl2 for the enantioselective acetal formation from N-propanoyl-1,3-thiazinane-2-thione and trimethyl orthoformate | - |
dc.type | info:eu-repo/semantics/article | - |
dc.type | info:eu-repo/semantics/acceptedVersion | - |
dc.identifier.idgrec | 718065 | - |
dc.date.updated | 2022-05-30T16:33:17Z | - |
dc.rights.accessRights | info:eu-repo/semantics/openAccess | - |
Appears in Collections: | Articles publicats en revistes (Institut de Biomedicina (IBUB)) Articles publicats en revistes (Química Inorgànica i Orgànica) |
Files in This Item:
File | Description | Size | Format | |
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718065.pdf | 10.1 MB | Adobe PDF | View/Open |
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