a method of making - 3 -- 5 - methylhexanoic acid that comprises condensing isovaleraldehyde with ## str1 ## to form primarily ## str2 ## reacting the ## str3 ## with a cyanide source to form ## str4 ## decarboxylating the ## str5 ## to form ## str6 ## hydrolyzing the ## str7 ## with an alkali or alkaline earth metal hydroxide to form an alkali or alkaline earth metal carboxylate salt ; and hydrogenating the alkali or alkaline earth metal carboxylate salt to form - 3 -- 5 - methylhexanoic acid , wherein r 1 and r 2 are the same or different and are hydrogen , c 1 - c 6 alkyl , aryl , benzyl , or c 3 - c 6 cycloalkyl . the present invention also provides a method of making - 3 -- 5 - methylhexanoic acid that comprises condensing isovaleraldehyde with ## str8 ## to form primarily ## str9 ## reacting the ## str10 ## with a cyanide source to form ## str11 ## decarboxylating the ## str12 ## to form an alkali or alkaline earth metal carboxylate salt ; and hydrogenating the alkali or alkaline earth metal carboxylate salt to form - 3 -- 5 - methylhexanoic acid .