Potassium Iodide → N-{4-[2-(4-Benzo[D]isothiazol-3-YL-piperazin-1-YL)-ethyl]-5-chloro-2-methyl-phenyl}-N-methyl-acetamide

N-[4-(2-chloro-ethyl)-2-methyl-phenyl]-N-methyl-acetamide (0.300 g, 1.153 mmol), 3-piperazin-1-yl-benzo[d]isothiazole hydrochloride (0.442 g, 1.729 mmol), potassium carbonate (0.237 g, 1.729 mmol), and potassium iodide (0.173 g, 1.153 mmol) in acetonitrile (3.5 mL) was subjected to 150° C. for 30 min. under microwave assistance using a Smith Personal Chemistry microwave. The reaction was diluted with H2O (50 mL) and CH2Cl2 (100 mL). The layers were separated and the organics washed with 1 N HCl (2×25 mL). The aqueous layer was made basic and extracted with CH2Cl2 (3×50 mL). The organics were dried (MgSO4), and concentrated to a solid residue. The residue was subjected to chromatography (MeOH:CH2Cl2 1:19) and collected as an amorphous residue and taken up in 1,4-dioxane and subjected to HCl gas for 10 min. The resulting solid was collected by filtration and dried at 50° C. under high vacuum overnight (0.770 g). 100% purity at 254 nm; LCMS (APCI): 409.2 [M+H]+.

1. customThe layers were separated
2. washthe organics washed with 1 N HCl (2×25 mL)
3. extractionextracted with CH2Cl2 (3×50 mL)
4. dry with materialThe organics were dried (MgSO4)
5. concentrationconcentrated to a solid residue
6. customcollected as an amorphous residue
7. filtrationThe resulting solid was collected by filtration
8. customdried at 50° C. under high vacuum overnight (0.770 g)

ORDレコード

ord-73ae26c538f24183a4240c2ef0326c38

出典データセット

uspto-grants-2006_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07101886B2