## Abstract Utilizing the facile acylative annulation of 2‐methoxypropene with [1‐^14^C]malonyl dichloride (5), the synthesis of 1,3,5‐trimethoxy[1‐^14^C]benzene (8) was accomplished through a seven‐step sequence starting from potassium [^14^C]cyanide with an overall yield of 60%. Thus, reaction o
Synthesis of 3,3-(14C)-dimethyl-1-phenyltriazene from 14C-dimethylamine hydrochloride and benzene-diazonium fluoroborate
✍ Scribed by G. F. Kolar; Ch. Schweickhardt
- Publisher
- John Wiley and Sons
- Year
- 1975
- Tongue
- French
- Weight
- 286 KB
- Volume
- 11
- Category
- Article
- ISSN
- 0022-2135
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✦ Synopsis
Abstract
3,3‐(^14^C)‐Dimethyl‐1‐phenyltriazene was prepared from recrystallized benzenediazonium fluoroborate which was coupled with ^14^C‐dimethylamine in excess aqueous sodium carbonate at 0°. The crude product was extracted with ether and purified by distillation. Redistilled ^14^C‐labelled triazene was obtained in good yield (70.4 and 73.5%) and in high radiochemical purity (better than 99.9% by scan of thin‐layer chromatograms). The specific activities of two preparations, determined by liquid scintillation counting and corrected for quenching, were 244 and 296 μCi/mmole. The determined activities were in close agreement with values computed from the specific activity of ^14^C‐dimethylamine hydrochloride used in the synthesis.
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