Process for the palladium-catalyzed amidation of vinyl chloride

Organic compounds -- part of the class 532-570 series – Organic compounds – Amino nitrogen containing

Patent

Rate now

  [ 0.00 ] – not rated yet Voters 0   Comments 0

Details

564205, C07C23110

Patent

active

051591138

ABSTRACT:
A unique two-step process is disclosed for the surprisingly high rate of amidation of vinyl chloride (VCl) with carbon monoxide and certain amines catalyzed by an effective amount of monodentate tertiary phosphonium complexes of Pd(0). The rate is orders of magnitude faster than that of other monochloroalkenes. When compared with the three chloropropenes, the simplest alkyl-substituted derivatives of VCl, rates differ by a factor of about 40 to 70 with ammonia as the amine. The reaction product with VCl is mainly the Michael adduct of the amine with the acrylamide produced. However, the chloroprenes give the propenamides with retention of configuration in the case of cis- and trans-1-chloropropene, and no adduct formation. The formation of this adduct has an important influence on catalyst stability since it can compete with the addition of the tertiary-phosphonium ligand from the catalyst complex. The latter reaction produces small amounts of a phosphonium chloride, and the resulting loss of ligand causes palladium metal to separate, thereby deactivating the catalyst. This understanding enables one to choose the best ligand/amine combination to suppress this catalyst deactivation mechanism. Triphenylphosphine and dimethylamine is a particularly effective combination.

REFERENCES:
patent: 3988358 (1976-10-01), Heck
patent: 3991101 (1976-11-01), Knifton
patent: 4128554 (1978-12-01), Heck
Mori et al., J. Org. Chem., 1983, 48, 4058-67.
Breinet et al., J. Org. Chem:, 1983, 48 1166-71.
Fitton et al., J. Organometallic Chem., 28 (1971), 287-91.
Ishii et al., J. Organometallic Chem., 73 (1974), 411-18.
Koketsu et al., Chubu Kogyo Daigaka, Kiyo, A. 16A, 103-9 (1980).
Johnson, et al., J. Chem Soc., (1974), 34-40.
Tolman, Chemical Reviews, 1977, vol. 77, No. 3, 313-48.
Heck et al., Catalysis in Organic Synthesis, Patel, 1978, 7th Ed. 195-218.
"Chelate-Assisted, Pd-Catalyzed Efficient Carbonylation of Aryl Chlorides" by Y. Ben-David, M. Portnoy and D. Milstein, J. Am. Chem. Soc. 1989 111, p. 8742-8744.
"Oxidative Addition of Water to the Ru.sup.11 Catalyst K[Ru.sup.11 (Hedta)CO)]: Homogeneous Catalysis of the Water-Gas Shift Reaction under Ambient Conditions."
"Palladium-Catalyzed Amidation of Aryl, Heterocyclic, and Vinylic Halides", by A. Schoenberg and R. F. Heck J. Org. Chem. vol. 39, No. 23, 1974 pp. 3327-3331.
"Amidation of Chloroalkenes Catalyzed by Tertiary Phosphine Complexes of Palladium (0)" by Paul P. Nicholas, J. Org. Chem. vol. 52, No. 23, 1987 pp. 5266-5272.

LandOfFree

Say what you really think

Search LandOfFree.com for the USA inventors and patents. Rate them and share your experience with other people.

Rating

Process for the palladium-catalyzed amidation of vinyl chloride does not yet have a rating. At this time, there are no reviews or comments for this patent.

If you have personal experience with Process for the palladium-catalyzed amidation of vinyl chloride, we encourage you to share that experience with our LandOfFree.com community. Your opinion is very important and Process for the palladium-catalyzed amidation of vinyl chloride will most certainly appreciate the feedback.

Rate now

     

Profile ID: LFUS-PAI-O-906773

  Search
All data on this website is collected from public sources. Our data reflects the most accurate information available at the time of publication.