반응 #1478067

반응 방정식

methyl 2-sulfoethyldithiocarbamate potassium salt

sodium azide

water

→

1-(2-sulfoethyl)-tetrazole-5-thiol

용매

acetone

반응 조건

후처리

1. 1
   workup.ADDITIONA mixture of 21.5 g
2. 2
   온도The solution was cooled to 25°
3. 3
   추출extracted with ethyl acetate
4. 4
   workup.ADDITIONThe aqueous phase was treated with Amberlite IR-120H resin
5. 5
   세척washed with ether
6. 6
   기타evaporated
7. 7
   기타to give an oil
8. 8
   여과the solution was filtered
9. 9
   기타the filtrate was evaporated to dryness

실험 절차

A mixture of 21.5 g. (0.087 mol.) of methyl 2-sulfoethyldithiocarbamate potassium salt (0.5 hydrate) and 7.16 g. (0.11 mol.) of sodium azide in 200 ml. of water was refluxed for two hours. The solution was cooled to 25° and extracted with ethyl acetate. The aqueous phase was treated with Amberlite IR-120H resin, washed with ether and evaporated to give an oil. The oil was dissolved in acetone, the solution was filtered and the filtrate was evaporated to dryness to give 1-(2-sulfoethyl)-tetrazole-5-thiol. The thiol was dissolved in isopropanol, cyclohexylamine was added until pH 8-9 and acetonitrile was added to give 1-(2-sulfoethyl)tetrazole-5-thiol as the di-cyclohexylamine salt.

출처