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ChemicalBook CAS DataBase List N-NITROSODI-N-HEXYLAMINE

N-NITROSODI-N-HEXYLAMINE synthesis

3synthesis methods
-

Yield:6949-28-6 96%

Reaction Conditions:

with N,N,N’,N’-tetrabromobenzene-1,3-disulfonamide;water;silica gel;sodium nitrite in dichloromethane at 20; for 0.05 h;Reagent/catalyst;

Steps:

General Procedure for N-nitrosation of Secondary Amineswith TBBDA and PBBS

General procedure: To a stirred solution of amine (1 mmol) in CH2Cl2 (5mL), NaNO2 (2 mmol), wet SiO2 (50% w/w, 0.2 g) andPBBS (0.5 g) or TBBDA (0.35 mmol) were added. The heterogeneousreaction mixture was stirred at room temperaturefor appropriate time (Table 2). After completion of the reaction[the reaction progress was monitored by TLC (nhexane:ethyl acetate 8:2)], the reaction mixture was filteredand washed with dichloromethane (25 mL). Then anhydrousNa2SO4 (2 g) was added and filtered off. Dichloromethanewas removed by reduced pressure and Nnitrosamineswere obtained (Table 2). For further purificationcolumn chromatography on silica gel (n-hexane:ethylacetate 8:2) was used.

References:

Ghorbani-Vaghei, Ramin;Shiri, Lotfi;Ghorbani-Choghamarani, Arash [Letters in Organic Chemistry,2013,vol. 10,# 3,p. 204 - 208]

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