反应详情

A suspension of 4-(cyclopropylmethyl)piperidine-4-carbonitrile hydrochloride (I-3, 2.5 g, 12.5 mmol) in CH2Cl2 (130 mL) at 0° C. was treated with i-Pr2NEt (8.7 mL, 50 mmol) and EtSO2Cl (1.8 mL, 18.7 mmol) dropwise. After 2 h, the reaction was quenched with the addition of 1 M aqueous NaOH (40 mL) and stirred 18 h before being extracted with CH2Cl2 (3×50 mL). The combined organic extracts were dried (Na2SO4) and concentrated under reduced pressure to afford 4-(cyclopropylmethyl)-1-(ethylsulfonyl)piperidine-4-carbonitrile (I-4, M+H+=256.1) as an off-white amorphous solid. This material was used in subsequent reactions without further purification.

1. customthe reaction was quenched with the addition of 1 M aqueous NaOH (40 mL)
2. extractionbefore being extracted with CH2Cl2 (3×50 mL)
3. dry with materialThe combined organic extracts were dried (Na2SO4)
4. concentrationconcentrated under reduced pressure