Di-π-methane rearrangement explained

In organic chemistry, the di-π-methane rearrangement is the photochemical rearrangement of a molecule that contains two π-systems separated by a saturated carbon atom. In the aliphatic case, this molecules is a 1,4-diene; in the aromatic case, an allyl-substituted arene. The reaction forms (respectively) an ene- or aryl-substituted cyclopropane. Formally, it amounts to a 1,2 shift of one ene group (in the diene) or the aryl group (in the allyl-aromatic analog), followed by bond formation between the lateral carbons of the non-migrating moiety:[1]

Discovery

This rearrangement was originally encountered in the photolysis of barrelene to give semibullvalene.[2] Once the mechanism was recognized as general by Howard Zimmerman in 1967, it was clear that the structural requirement was two π groups attached to an sp3-hybridized carbon, and then a variety of further examples was obtained.

Notable examples

One example was the photolysis of Mariano's compound, 3,3dimethyl-1,1,5,5tetraphenyl-1,4pentadiene. In this symmetric diene, the active π bonds are conjugated to arenes, which does not inhibit the reaction.[3] [4] [5]

Another was the asymmetric Pratt diene. Pratt's diene demonstrates that the reaction preferentially cyclopropanates aryl substituents, because the reaction pathway preserves the resonant stabil­ization of a benzhydrylic radical inter­mediate.[6]

The barrelene rearrangement is more complex than the Mariano and Pratt examples since there are two sp3-hybridized carbons. Each bridgehead carbon has three (ethylenic) π bonds, and any two can undergo the diπ-methane rearrangement. Moreover, unlike the acyclic Mariano and Pratt dienes, the barrelene reaction requires a triplet excited state. Thus acetone is used in the barrel­ene reaction; acetone captures the light and then delivers triplet excitation to the barrelene reactant. In the final step of the rearrangement there is a spin flip, to provide paired electrons and a new σ bond.

As excited-state probe

The dependence of the di-π-methane re­arrange­ment on the multiplicity of the excited state arises from the free-rotor effect.[7] Triplet 1,4-dienes freely undergo cis-trans inter­conversion of diene double bonds (i.e. free rotation). In acyclic dienes, this free rotation leads to diradical reconnection, short-circuiting the di-π-methane process. Singlet excited states do not rotate and may thus undergo the di-π-methane mechanism. For cyclic dienes, as in the barrelene example, the ring structure can prevent free-rotatory dissipation, and may in fact require bond rotation to complete the rearrangement.

References

  1. Synthetic Aspects of the Di--methane Rearrangement. 10.1021/cr910109c . 11848853 . 1996 . Zimmerman . Howard E. . Armesto . Diego . Chemical Reviews . 96 . 8 . 3065–3112.
  2. Zimmerman . H. E. . Grunewald . G. L. . 1966 . The Chemistry of Barrelene. III. A Unique Photoisomerization to Semibullvalene . J. Am. Chem. Soc. . 88 . 1. 183–184 . 10.1021/ja00953a045 .
  3. Zimmerman. Howard E.. Binkley. Roger W.. Givens. Richard S.. Sherwin. Maynard A.. Mechanistic organic photochemistry. XXIV. The mechanism of the conversion of barrelene to semibullvalene. A general photochemical process. Journal of the American Chemical Society. 89. 15. 1967. 3932–3933. 0002-7863. 10.1021/ja00991a064.
  4. Zimmerman . H. E. . Mariano . P. S . 1969 . The Di--methane Rearrangement. Interaction of Electronically Excited Vinyl Chromophores . J. Am. Chem. Soc. . 91 . 1718–1727 . 10.1021/ja01035a021.
  5. The Di--methane and Oxa-di--methane rearrangements. 10.1021/cr60285a005 . 1973 . Hixson . Stephen S. . Mariano . Patrick S. . Zimmerman . Howard E. . Chemical Reviews . 73 . 531 . 5.
  6. Zimmerman . H. E. . Pratt . A. C . 1970 . Unsymmetrical Substitution and the Direction of the Di--methane Rearrangement; Mechanistic and Exploratory Organic Photochemistry. LVI . J. Am. Chem. Soc. . 92 . 6259–6267 . 10.1021/ja00724a026.
  7. Zimmerman . H. E. . Schissel . D. N . 1986 . Di--methane Rearrangement of Highly Sterically Congested Molecules: Inhibition of Free Rotor Energy Dissipation. Mechanistic and Exploratory Organic Photochemistry . J. Org. Chem. . 51 . 196–207 . 10.1021/jo00352a013.