Azobisisobutyronitrile → HCID 67721486, compound

Participants

Reaction Steps

The compound 116 obtained above (7.27 g, 12.5 mmole) was dissolved in benzene (40 ml), and 5-mercapto-1-methyltetrazole disulfide (2.88 g, 12.5 mmole) and α,α'-azobis-isobutyronitrile (205 mg, 1.25 mmole) were added thereto, and the mixture was refluxed with stirring for 19 hours. Then, the reaction mixture was treated following the procedure similar to that of Example 41, to yield a residue. The residue was chromatographed over silica gel (330 g), eluting with ethyl acetate: n-hexane (1:50), to yield 5.34 g of a mixture of geometrical isomers with respect to the double bond. The material was further chromatographed over 10% silver nitrate--silica gel (500 g), eluting with ether-n-hexane (1:50), to yield 3.64 g of the title compound 117 (yield 50%).

Provenance & Evidence