反应详情

Phosphoric acid (11.40 mL, 196 mmol) was added to a flask containing water (500 mL). The solution was stirred for about 5 min. (1S,2R,4S)-4-(dibenzylamino)-2-methylcyclopentanecarboxylate•(R)-1-phenylethanamine (83 g, 187 mmol) was added to the solution in small portions. MTBE (500 mL) was added and the contents were mixed well, dissolving the solid. The phases were settled and separated. The aqueous layer was back extracted with MTBE (150 mL). The combined organic phases were dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to afford (1S,2R,4S)-4-(dibenzylamino)-2-methylcyclopentanecarboxylic acid (60 g, 99%) as an oil: HPLC (Table 1, Method x) Rt=4.57 min.

1. additionwas added to the solution in small portions
2. additionthe contents were mixed well
3. dissolutiondissolving the solid
4. customseparated
5. extractionThe aqueous layer was back extracted with MTBE (150 mL)
6. dry with materialThe combined organic phases were dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo