Morpholine → 4-[5-Morpholin-4-yl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester

온도

100 °C

A mixture of 4-[5-(nonafluorobutane-1-sulfonyloxy)-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (200 mg, 0.286 mmol) produced in Example (81c), morpholine (37.8 mg, 0.429 mmol), sodium t-butoxide (56.7 mg, 0.572 mmol), tris(dibenzylideneacetone)dipalladium(0) (13.1 mg, 0.0143 mmol), 2-dicyclohexylphosphino-2′-(N,N-dimethylamino)biphenyl (11.5 mg, 0.0286 mmol) and xylene (3 mL) was stirred for 13 hours and 30 minutes at an external temperature of 100° C. under a nitrogen atmosphere. The reaction mixture was filtered through Celite to remove insoluble materials, and the filtrate was concentrated under reduced pressure. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 103 mg of the title compound as a light yellow oil.

1. filtrationThe reaction mixture was filtered through Celite
2. customto remove insoluble materials
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane)

ORD 기록

ord-63076f28cfe141b6969d24a81bc62a90

출처 데이터셋

uspto-grants-2008_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07410971B2