Reactivity of Ru(H)(H2)Cl(PCy3)2 with propargyl and vinyl chlorides: New methodology to give metathesis-active ruthenium carbenes

Organometallics

Volumn 16, Issue 18, 1997, Pages 3867-3869

  Wilhelm, Thomas E ^a   Belderrain, Tomás R ^a   Brown, Seth N ^a   Grubbs, Robert H ^a  

^a California Institute of Technology ^*  (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 33646142047     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om9705259     Document Type: Article

References (25)

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22. x (3) (4.00 g, 14.28 mmol) and tricyclohexylphosphine (Strem, 97% pure, 8.46 g, 29.26 mmol) were placed in a 500 mL high-pressure system equipped with a pressure gauge. To this system, 200 mL of degassed sec-butyl alcohol and triethylamine (1.99 mL, 14.28 mmol) were added. After purging with hydrogen, the system was pressurized with 1.5 atm of hydrogen and heated to 80 °C for a total of 20 h, repressurizing as needed. Generation of (1) can also be accomplished in a suitably-sized, thickwalled Teflon-valved Straus flask. The air-sensitive orange solid was isolated by cooling the system to room temperature, adding a volume (200 mL) of degassed methanol to ensure complete precipitation before filtering, washing with methanol (3 × 50 mL), and drying in vacuo to give 9.26 g, 94% of 1.
23. 2. Noncommercially available alkynes were made following the procedures in a Brandsma, L. Preparative Acetylenic Chemistry; Elsevier. Amsterdam, 1988.
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