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ChemicalBook CAS DataBase List 3,4-Diaminothiophene dihydrobromide
78637-85-1

3,4-Diaminothiophene dihydrobromide synthesis

3synthesis methods
-

Yield: 94%

Reaction Conditions:

with [Cu2(2,7-bis(pyridin-2-yl)-l,8-naphthyridine)(OH)(CF3COO)3];tetrabutylammomium bromide;ammonia;caesium carbonate in ethylene glycol at 140; for 16 h;Sealed tube;chemoselective reaction;

Steps:

2.2 General procedure for amination
General procedure: A mixture of substrate (0.25 mmol), complex 1 (2.5 × 10- 3 mmol), Cs2CO3 (1 mmol), Conc. NH3(aq) (0.5 mL) and TBAB (0.25 mmol) in water (0.5 mL) were loaded in a sealed reaction tube. The reaction temperature was increased to 110-140 °C and the reaction mixture was stirred for 8-24 h. After cooling to RT, the reaction mixture was poured into a saturated NaCl solution, extracted with ethyl acetate and dried over anhydrous MgSO4. After removal of solvents, the residue was re-crystallized or chromatographed on silica gel. All products were characterized by NMR spectroscopy and were consistent with the literature data.

References:

Liao, Bei-Sih;Liu, Shiuh-Tzung [Catalysis Communications,2013,vol. 32,p. 28 - 31]

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