反应详情

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 4-(4-amino-pyrazol-1-ylmethyl)-thiazole-2-carboxylic acid ethyl ester (1.43 g, 5.65 mmol) in CH2Cl2 (56.0 mL) was treated with DIPEA (1.15 mL, 8.47 mmol) followed by 2-chlorobenzylchloroformate (1.04 mL, 6.78 mmol). The reaction mixture was stirred at rt for 1 h before being quenched with water (50 mL), extracted with CH2Cl2 (3×40 mL). The combined org. extracts were dried over MgSO4, filtered, and the solvent was removed under reduced pressure. Purification of the residue by FC (96:4 CH2Cl2-MeOH) gave the title compound as a pink foam. TLC: rf (96:4 CH2Cl2-MeOH)=0.28. LC-MS-conditions 02: tR=0.99 min; [M+H]+=421.14.

1. custombefore being quenched with water (50 mL)
2. extractionextracted with CH2Cl2 (3×40 mL)
3. dry with materialextracts were dried over MgSO4
4. filtrationfiltered
5. customthe solvent was removed under reduced pressure
6. customPurification of the residue by FC (96:4 CH2Cl2-MeOH)