Dimethyl Sulfoxide → N-(2-methyl-1,3-benzoxazol-6-yl)-4-(4-phenyl-1,3-thiazol-2-yl)piperazine-1-carboxamide

A solution of 2,2,2-trichloroethyl (2-methyl-1,3-benzoxazol-6-yl)carbamate (200 mg, 0.618 mmol), 1-(4-phenyl-1,3-thiazol-2-yl)piperazine (152 mg, 0.618 mmol), diisopropylethylamine (0.215 ml, 1.24 mmol) and dimethyl sulfoxide (4 ml) was stirred at 70° C. for 24 hours, and the reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with water, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to give the desired product as a solid. The solid was recrystallized from ethyl acetate to give 100 mg (38.6%) of the desired product as a solid.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationThe solvent was distilled off under reduced pressure
5. customThe residue was purified by silica gel column chromatography (ethyl acetate)

ORDレコード

ord-567c3d0f9d0047adb7fe943c29f79cde

出典データセット

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07851473B2