반응 #60493
ord-dfe99c3ce2a543f192d80bfdd4dfe622
반응 방정식
반응물
시약
반응 조건
후처리
- 1기타During the reaction
- 2기타the 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
- 4온도The reaction mixture was cooled to room temperature
- 5추출extraction
- 6추출The aqueous layer was again extracted with chloroform
- 7세척washed with brine
- 8건조dried over anhydrous magnesium sulfate
- 9여과The desiccant was filtered off
- 10농축the filtrate was concentrated under reduced pressure
- 11기타The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane)
실험 절차
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.