反应详情

To a solution of 100.0 g N-(1-methylethyl)-2,3-dimethyl-2-butylamine in 200 mL ethanol, 100 mL hydrochloric acid was added with shaking and cooling in an glacial water bath. The solvent was distilled off to dry in vacuum. The residue was dissolve in ethanol, then distilled off to dry in vacuum and crystallized from 1:1 i-PrOH-c-Hex-H to give a solid 130.5 g (95.5%), mp 228-230° C.(i-PrOH:Et2O). Elemental analysis for C9H22ClN(%): Calculated C, 60.14; H, 12.34; N, 7.79; Cl, 19.73. Found C, 60.14; H, 12.48; N, 7.31; Cl, 19.67. 1H-NMR (D2O, ppm) 0.98(d, J=6.75H, 6H), 1.33(s, 6H), 1.37(d, J=6.46, 6H), 2.10(m, 1H), 3.70(m, 1H). MS(m/z) 143(M+), 100(B).

1. temperaturecooling in an glacial water bath
2. distillationThe solvent was distilled off
3. customto dry in vacuum
4. dissolutionThe residue was dissolve in ethanol
5. distillationdistilled off
6. customto dry in vacuum
7. customcrystallized from 1:1 i-PrOH-c-Hex-H