تفاعل #60482

معادلة التفاعل

4-[5-(nonafluorobutane-1-sulfonyloxy)-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester

morpholine

sodium t-butoxide

2-dicyclohexylphosphino-2′-(N,N-dimethylamino)biphenyl

→

title compound

المردود 74.1%

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

المردود 74.1%

المذيبات

xylene

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر