反应详情

温度

120 °C

2-(Chloromethyl)-1-(3,5-dichlorobenzyl)-1H-imidazole hydrochloride (see Example 1) (100 mg, 0.32 mmol), cyclohexanol (160 mg, 1.6 mmol) and acetonitrile (1 mL) were combined in a Smith Process Vial. The reaction mixture was heated in a SmithSynthesizer™ (Personal Chemistry) microwave at 120° C. for 30 min. The heterogeneous solution was filtered and the solid was washed with acetonitrile. The filtrate was concentrated and the resulting semi-solid was partitioned between CH2Cl2 (10 mL) and 5% Na2CO3 (5 mL). The aqueous layer was extracted with CH2Cl2 (2×10 mL). The combined organic layers were dried over MgSO4, filtered and concentrated to afford the desired product (11 mg, 10%); MS m/z 339 [C17H20Cl2N2O+H]+.

1. filtrationThe heterogeneous solution was filtered
2. washthe solid was washed with acetonitrile
3. concentrationThe filtrate was concentrated
4. customthe resulting semi-solid was partitioned between CH2Cl2 (10 mL) and 5% Na2CO3 (5 mL)
5. extractionThe aqueous layer was extracted with CH2Cl2 (2×10 mL)
6. dry with materialThe combined organic layers were dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated