Reaction #1177229
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04005218
Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: A mixture of 40 parts of 4-chloro-α-[2-chloro-4-(hydroxyimino)-5-methyl-2,5-cyclohexadien-1-ylidene]benzeneacetonitrile, 50 parts of iron-powder, 1500 parts of ammonium chloride solution 0.78N and 270 parts of methylbenzene is stirred and refluxed overnight. The reaction mixture is filtered over hyflo and the filter-cake is washed with 4-methyl-2-pentanone. The filtrate is dried, filtered and evaporated. The solid residue is crystallized from methylbenzene. The product is filtered off and recrystallized from methylbenzene, yielding 4-amino-2-chloro-α-(4-chlorophenyl)-5-methylbenzeneacetonitrile; mp. 152.6° C. refluxed overnight The reaction mixture is filtered over hyflo the filter-cake is washed with 4-methyl-2-pentanone The filtrate is dried filtered evaporated The solid residue is crystallized from methylbenzene The product is filtered off recrystallized from methylbenzene
Source ID: ord-126b345fdc694b8ebbc98f895108ff60