تفاعل #60493
ord-dfe99c3ce2a543f192d80bfdd4dfe622
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1أخرىDuring the reaction
- 2أخرىthe excess hydrogen chloride gas in the reactor was removed several times with nitrogen gas
- 3workup.STIRRINGthe mixture was stirred for 1 hour under the same conditions
- 4درجة الحرارةThe reaction mixture was cooled to room temperature
- 5استخلاصextraction
- 6استخلاصThe aqueous layer was again extracted with chloroform
- 7غسيلwashed with brine
- 8تجفيفdried over anhydrous magnesium sulfate
- 9ترشيحThe desiccant was filtered off
- 10تركيزthe filtrate was concentrated under reduced pressure
- 11أخرىThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane)
الإجراء التجريبي
A mixture of the crude product of 4-methoxy-2-(3,3,5,5-tetramethylcyclohexyl)phenylamine produced in Example (85b), bis(2-chloroethyl)amine hydrochloride (770 mg, 4.33 mmol) and 1,2-dichlorobenzene (10 ml) was stirred for 2 hours at an external temperature of 220° C. During the reaction, the excess hydrogen chloride gas in the reactor was removed several times with nitrogen gas. Bis(2-chloroethyl)amine hydrochloride (180 mg, 1.01 mmol) was then added and the mixture was stirred for 1 hour under the same conditions. The reaction mixture was cooled to room temperature, saturated aqueous solution of sodium hydrogencarbonate was added and extraction was performed with chloroform. The aqueous layer was again extracted with chloroform, and the organic layers were combined, washed with brine and then dried over anhydrous magnesium 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/heptane) to give 660 mg of the title compound as a brown solid.