The process for preparation of and the intermediate compounds such as 1H-tetrazole-5-thiol having the formula ##STR1## wherein R.sub.1 is alkyl, aminoalkyl, acylaminoalkyl, aryl, alkoxycarbonylaminoalkyl, halogen-substituted aryl or alkylamino-substituted aryl and R.sub.2 is hydrogen or arakyl, preferably benzyl. The compound is produced by reacting a substituted thiosemicarbazide with an aralkyl chloride, subjecting the resultant compound to diazotization, and reacting the resultant compound with a Friedel Crafts catalyst. Optionally, this may be further hydrolyzed when R.sub.1 is aminoalkyl and/or converted to conventional salts.