Procedure for the industrial obtaining of 1, 2, 3, 4, 10, 10-hexachloro-1, 4, 4a, 5, 8, 8a hexahidro-1, 4, 5, 8-bisensometilennaftaleno (empire formula c12 h8 ocl6) (Machine-translation by Google Translate, not legally binding)

摘要

Process for the industrial preparation of 1,2,3,4,10,10-hexachloro-1,4,4a, 5,8,8a hexahydro-1,4,5,8-endomethylene-naphthalene (empirical formula C12H8Cl6) and 1,2,3,4,10,10-hexachloro 6,7-epoxy-1,4,4a, 5,6,7,8,8a-octahydro-1,4,5,8-bisendomethylene-naphthalene (formula empirical C12H8OCl6), characterized in that equal parts of bicyclo- (2,2,1) -2,5-heptadiene (8.16 moles) and hexachlorocyclopentadiene (2.74 moles) are mixed and heated, keeping for 16 a 18 hours at 85-90º C in a vacuum of 630 m/m in the reflux condenser. After this time the starting products are distilled in excess. The residue is still distilled at 20 m/m until the temperature reaches 125º C in the reaction vessel. The residue solidifies upon cooling and corresponds approximately to the theoretical yield of the Diels-Alder adduct. It is distilled at 1 m/m vacuum obtaining 786 g of distilled product of P.F./1mm: 132-150ºC. The crude 1,2,3,4,10,10-hexachloro-1,4,4a, 5,8,8a hexahydro-1,4,5,8-endomethylene-naphthalene is recrystallized from a mixture of acetone and methanol 1: 2.5 (parts of volume). Approximate performance; 36%, white needles P.F. 101-104º C. (Machine-translation by Google Translate, not legally binding)