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ChemicalBook CAS DataBase List Sodium bicarbonate
144-55-8

Sodium bicarbonate synthesis

10synthesis methods
Sodium bicarbonate is manufactured either by passing carbon dioxide into a cold saturated solution of sodium carbonate, or by the ammonia–soda (Solvay) process, in which first ammonia and then carbon dioxide is passed into a sodium chloride solution to precipitate sodium bicarbonate while the more soluble ammonium chloride remains in solution.
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Yield:227626-62-2 80%

Reaction Conditions:

in ice-water;N,N-dimethyl-formamide;

Steps:

4 (1-Cyanomethyl-cyclohexylmethyl)-carbamic acid tert-butyl ester (4)

(1-Cyanomethyl-cyclohexylmethyl)-carbamic acid tert-butyl ester (4) Cyanuric chloride (39.5 g, 0.214 mol) was added to (1-carbamoylmethyl-cyclohexylmethyl)-carbamic acid tert-butyl ester (3) (116 g, 0.429 mol) in 400 mL DMF. An ice-water bath was used to moderate the exotherm, and the reaction mixture was stirred at room temperature for 1.5 hours. The mixture was poured into ice-water containing 120 g (1.43 mol) NaHCO3 and was extracted 4*EtOAc. The extracts were washed 1*water, 2* brine and dried over Na2SO4. Evaporation yielded an oil which was taken up in 3:1 hexane/EtOAc and filtered through silica gel. Evaporation yielded white crystals (86.5 g, 80%); mp 54-58° C. 1H-NMR (CDCl3) δ1.3-1.5 (m, 19H), 2.30 (s, 2H), 3.15 (d, 2h, J=7.00 Hz), 4.60 (broad, 1H). MS (APCI) m/z 253 (M+1).

References:

US6518289,2003,B1

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