N,N-bis(2-methoxyethyl)sulfamoyl chloride

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A premixed solution of bis-methoxyethylamine (15.0 ml, 102 mmol, 1.00 equiv.) and triethylamine (21.3 ml, 153 mmol, 1.50 equiv.) was added dropwise to a solution of sulfuryl chloride (20.7 ml, 153 mmol, 1.50 equiv.) in CH2Cl2 at 0° C. The reaction mixture was continued stirred at 0° C. for 2 h, poured into ice and extracted with CH2Cl2 (3×100 ml). The combined organic extracts were washed with a saturated NaCl soln (1×100 ml), the organic layer dried (Na2SO4), filtered and concentrated under vacuum to afford the title compound (18.5 g, 80%) which was used without further purification. 1HNMR (CDCl3): 3.37 (s, 6H), 3.64-3.64 (m, 8H) poured into ice extracted with CH2Cl2 (3×100 ml) The combined organic extracts were washed with a saturated NaCl soln (1×100 ml) the organic layer dried (Na2SO4) filtered concentrated under vacuum

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A premixed solution of bis-methoxyethylamine (15.0 ml, 102 mmol, 1.00 equiv.) and triethylamine (21.3 ml, 153 mmol, 1.50 equiv.) was added dropwise to a solution of sulfuryl chloride (20.7 ml, 153 mmol, 1.50 equiv.) in CH2Cl2 at 0° C. The reaction mixture was continued stirred at 0° C. for 2 h, poured into ice and extracted with CH2Cl2 (3×100 ml). The combined organic extracts were washed with a saturated NaCl soln (1×100 ml), the organic layer dried (Na2SO4), filtered and concentrated under vacuum to afford the title compound (18.5 g, 80%) which was used without further purification. 1HNMR (CDCl3): 3.37 (s, 6H), 3.64-3.64 (m, 8H) poured into ice extracted with CH2Cl2 (3×100 ml) The combined organic extracts were washed with a saturated NaCl soln (1×100 ml) the organic layer dried (Na2SO4) filtered concentrated under vacuum