反应详情

温度

50 °C

A mixture of Ethyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl) methyl]cyclobutanecarboxylate (4.2 g, 11.9 mmol, Step 5), 2N NaOH (18 mL) and EtOH (12 mL) was heated at 50° C. for 4 hrs. The resulting solution was cooled in ice bath and 2N HCl (ca 19 mL) was added until pH of the mixture was ca 5-6. The whole was extracted with CH2Cl2/iPrOH (3:1, 30 mL×3). Combined organic layer was dried (Na2SO4) and filtered. The filtrate was concentrated to give 3.8 g (98%) of the titled compound as yellow solid.

1. temperatureThe resulting solution was cooled in ice bath
2. extractionThe whole was extracted with CH2Cl2/iPrOH (3:1, 30 mL×3)
3. dry with materialCombined organic layer was dried (Na2SO4)
4. filtrationfiltered
5. concentrationThe filtrate was concentrated