반응 #477941

반응 방정식

compound

(2-chloro-5-(trifluoromethyl)benzyl)(3,5-bis(trifluoromethyl)benzyl)cyanamide

triethanolamine

trimethyl silyl azide

→

desired compound

수율 85.0%

N-(2-chloro-5-(trifluoromethyl)benzyl)-N-(3,5-bis(trifluoromethyl)benzyl)-1H-tetrazol-5-amine

수율 85.0%

용매

sodium hydroxide

반응 조건

후처리

1. 1
   온도the reaction mixture was cooled
2. 2
   기타The layers were separated
3. 3
   세척the organic layer washed with 50 mL of 10% citric acid
4. 4
   농축The organic layer was concentrated
5. 5
   기타triturated with hexane

실험 절차

A solution of 5 gm of the compound from Step C, 50 mL of 2-methyl THF 5 mL, triethanolamine and 2.5 mL of trimethyl silyl azide was heated at 50° C. until reaction completion. When the reaction was judged complete, the reaction mixture was cooled and 50 mL of 1 N sodium hydroxide added. The layers were separated and the organic layer washed with 50 mL of 10% citric acid. The organic layer was concentrated and triturated with hexane to yield 4.6 of the desired compound. 85% yield. 1H NMR (400 MHz, CDCl3) 7.84 (s, 2H), 7.74 (m, 3H), 4.90 (s, 4H)C, H, N, Calculated, (found) 42.92 (42.98), 2.20 (1.97), 13.90 (13.54)

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