反応 #60493
ord-dfe99c3ce2a543f192d80bfdd4dfe622
反応方程式
反応物
試薬
反応条件
後処理
- 1その他During the reaction
- 2その他the 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
- 4温度The reaction mixture was cooled to room temperature
- 5抽出extraction
- 6抽出The aqueous layer was again extracted with chloroform
- 7洗浄washed with brine
- 8乾燥dried over anhydrous magnesium sulfate
- 9ろ過The desiccant was filtered off
- 10濃縮the filtrate was concentrated under reduced pressure
- 11その他The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane)
実験手順
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.