Yield:736182-77-7 1.47 g

Reaction Conditions:

with sodium carbonate;sodium iodide in 1,4-dioxane at 70; for 24 h;

Steps:

Synthesis of 3-morpholinopropane-1-sulfonamide S10

As an alternative preparation of S10, 3 -chloropropane-1-sulfonamide (3.15 g, 20.0 mmol), morpholine (1.84, 21.0 mmol), sodium carbonate (4.24 g, 40.0 mmol) and sodium iodide (300 mg, 2.0 mmol) were heated in anhydrous dioxane (70 mL) at 70 °C for a day. The suspension was permitted to cool towards room temperature and then filtered through diatomaceous earth with an MTBE rinse. The filtrate was concentrated and chromatographed on silica (0 to 4% concentrated aqueous NH₄OH/CH₃CN) to give the titled compound (1.47 g). 1H NMR (400 MHz, CDCl₃) δ ppm 5.41 (s, 2H), 3.70 (t, J = 4.7 Hz, 4H), 3.23 (t, J = 7.2 Hz, 2H), 2.54-2.43 (m, 6H), 2.10-2.02 (m, 2H); MS (DCI) m/z 209 (M+H)⁺.

References:

WO2017/60874,2017,A1 Location in patent:Paragraph 00708