反应详情

温度

200 °C

To a mixture of 3-methyl-2-(3,3,5,5-tetramethylcyclohex-1-enyl)phenylamine (663 mg, 2.72 mmol) produced in Example (71b) and 1,2-dichlorobenzene (3 mL) was added bis(2-chloroethyl)amine hydrochloride (632 mg, 3.54 mmol), followed by stirring for 5 hours and 50 minutes at an external temperature of 200° C. under a nitrogen atmosphere. During the reaction, a nitrogen stream was passed through the reactor several times. The reaction mixture was cooled to room temperature, chloroform and saturated solution of sodium hydrogencarbonate were added, and the filtrate obtained by filtration through Celite was extracted with chloroform. The separated organic layer was washed with brine and then dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 625 mg of the title compound as a yellow solid.

1. customDuring the reaction
2. temperatureThe reaction mixture was cooled to room temperature
3. customthe filtrate obtained by filtration through Celite
4. extractionwas extracted with chloroform
5. washThe separated organic layer was washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationThe desiccant was filtered off
8. concentrationthe filtrate was concentrated under reduced pressure
9. customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane)