反应详情

To a solution of compound 23 (as per Example S above) (19 mg, 0.048 mmol, leg), NaBH3CN (6.0 mg, 0.096 mmol. 2 eq), NaBH(OAc)3 (31 mg, 0.144 mmol, 3 eq), NaOAc (15.7 mg, 0.19 mmol, 4 eq) in a mixture of anhydrous CH2Cl2 (2 mL), MeOH (2 mL) and DMF (0.5 mL) was added cyclopropylmethyl-methyl-amine hydrochloride (23 mg, 0.19 mmol, 4 eq) under Ar(g). The reaction mixture was stirred at rt overnight. Solvents were removed in vacuo. Then, the residue was partitioned with H2O (10 mL) and extracted with CH2Cl2 (3×10 mL) and EtOAc (2×10 mL). The combined organic extracts were dried over MgSO4 and the solvent was removed in vacuo. The residue was further purified by silica gel column chromatography with CH2Cl2/MeOH (1:0-47:3) to yield the product, T, as a white solid (8.35 mg, 37%).

1. customSolvents were removed in vacuo
2. customThen, the residue was partitioned with H2O (10 mL)
3. extractionextracted with CH2Cl2 (3×10 mL) and EtOAc (2×10 mL)
4. dry with materialThe combined organic extracts were dried over MgSO4
5. customthe solvent was removed in vacuo
6. customThe residue was further purified by silica gel column chromatography with CH2Cl2/MeOH (1:0-47:3)
7. customto yield the product, T