Unexpected Pyrolytic Behaviour of Substituted Benzo[c]thiopyran and Thieno[2,3-c]thiopyran S,S-dioxides

2014 ◽  
Vol 67 (9) ◽  
pp. 1288 ◽  
Author(s):  
R. Alan Aitken ◽  
Clémence Hauduc ◽  
M. Selim Hossain ◽  
Emily McHale ◽  
Adrian L. Schwan ◽  
...  

Flash vacuum pyrolysis (FVP) of benzo[c]thiopyran S,S-dioxide (1) results in formation of indene and 2-vinylbenzaldehyde as previously described. A range of eight analogues with various substitution patterns are found to behave differently. In general, there is no extrusion of SO2 to give products analogous to indene, but unsaturated carbonyl products analogous to 2-vinylbenzaldehyde are formed in most cases by way of ring expansion to a 7-membered ring sultine, extrusion of SO, and intramolecular hydrogen atom transfer. Other processes observed include formation of anthracene via an isomeric 7-membered sultine with loss of SO, CO and methane or butane, and formation of 4-ethylidene-4,5-dihydrocyclobuta[b]thiophenes by way of SO loss, a radical rearrangement, and extrusion of acetone. The analogues with a halogen substituent at position 8 on the benzene ring require a higher temperature to react and give naphthalene resulting from net elimination of HX and SO2. The X-ray crystal structure of 1 is also reported.

1998 ◽  
Vol 51 (10) ◽  
pp. 925 ◽  
Author(s):  
Jabbar Khalafy ◽  
Rolf H Prager

The flash vacuum pyrolysis products of 2-(benzotriazol-1-ylmethyl)benzonitrile, methyl 2-(benzotriazol-1-ylmethyl)benzoate and the corresponding benzisoxazolones have been characterized. The benzotriazoles lose nitrogen to give diradicals which undergo intramolecular hydrogen-atom transfer or cyclization, while the benzisoxazolones rearrange initially to the corresponding benzaldehyde N-(2-carboxyphenyl)imines which undergo subsequent intramolecular addition reactions.


1987 ◽  
Vol 40 (10) ◽  
pp. 1687 ◽  
Author(s):  
RFC Brown ◽  
KJ Coulston ◽  
BJ Dobney ◽  
FW Eastwood ◽  
GD Fallon

7-Methyl-1 H- indenone was trapped as the cyclopentadiene adduct endo* 8-methyl-1,4,4a,9a tetrahydro-1,4-methano-9H-fluoren-9-one (11) which was converted into the E- and Z-isomers (15) and (16) of endo (8'-methyl-l',4',4a',9a'-tetrahydro-1',4'-methano-9'H-fluoren-9'-ylidene) ethanoic acid by addition of methoxyethyne, rearrangement and hydrolysis. Both acids yielded the anhydride (17) of the E-acid on treatment with trifluoroacetic anhydride. Flash vacuum pyrolysis of this anhydride at 650� gave acenaphthylen-4-ol. 7-Methyl-1 H- indenylideneethenone (7) is proposed as an intermediate in this reaction and the results are discussed in relation to the rearrangement described in the title. The X-ray crystal structure of methyl endo (E)-(8'-methyl-l',4',4a',9a'-tetrahydro-l',4'-methano-9'H-fluoren-9'-ylidene) ethanoate (13) is reported.


1990 ◽  
Vol 43 (4) ◽  
pp. 765 ◽  
Author(s):  
AD Abell ◽  
KB Morris ◽  
V Mckee

An X-ray crystal structure and 1H n.m.r. analysis of the biphenyl phosphorane (4a) has revealed the presence of an intramolecular hydrogen bond resulting in an unusual biphenyl with a bridge forming a nine- membered ring. The related biphenyl phosphorane (4b) exists as two diastereoisomers.


2005 ◽  
Vol 60 (1) ◽  
pp. 33-36 ◽  
Author(s):  
Pritha Talukder ◽  
Amitabha Datta ◽  
Samiran Mitra ◽  
Georgina Rosair

A new one-dimensional coordination polymer [Co(CCl3COO)2(CH3OH)2(μ-4,4’-bipy)]n (1), has been synthesised and its crystal structure determined by single-crystal X-ray diffraction. The structure consists of a one-dimensional linear chain of cobalt(II) centres linked by bridging 4,4’-bipyridine units. The Co(II) ion lies at an inversion centre forming an elongated octahedral coordination sphere. There is an intramolecular hydrogen bond [2.02(5) Å ] between a trichloroacetate oxygen and a methanolic hydrogen forming a planar six-membered ring.


1994 ◽  
Vol 47 (6) ◽  
pp. 991 ◽  
Author(s):  
RFC Brown ◽  
FW Eastwood ◽  
GD Fallon ◽  
SC Lee ◽  
RP Mcgeary

Flash vacuum pyrolysis of 1-(alkyn-2′-oyl)-3-methylpyrazoles at 650°/0.03 mm forms pyrazolo[1,5-a]pyridin-5-ols, often in high yield, which may bear substituents at C2, C3 or C7. In the absence of a 3-methyl group in the precursor, N-ethynylpyrazoles are formed in low yield. The formation of both types of product is interpreted as involving 3-(N-pyrazolyl)propadienones formed by N1 → N2 migration of the N-alkynoyl group with inversion of the three-carbon chain. The fused-ring structure of 2-methylpyrazolo[1,5-a]pyridin-5-ol (25) was established by X-ray crystallography of the O-benzoyl derivative (27).


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