反应详情

温度

0 °C

A 250 mL, two-neck flask fitted with an addition funnel and thermocouple probe was charged with 1-cyclopropyl-piperazine dihydrochloride (7.1 g, 0.036 mol, 1.0 eq) and toluene (70 mL) and then cooled to 0° C. Aqueous NaOH solution (1.0 M, 70 mL, 2.0 eq) was added at such a rate that the reaction temperature did not exceed 10° C. Na2CO3 powder (7.5 g, 0.071 mol, 2.0 eq) was then added to the reaction mixture. The 4-morpholin-4-ylmethyl-benzoyl chloride, prepared as in Step A above (9.8 g, 0.036 mol, 1.0 eq) was added in portions over 3 minutes, while the temperature of the reaction mixture was maintained below 5° C. The reaction mixture was then stirred for 2 hrs. The reaction mixture was filtered, the layers were separated, the aqueous layer was extracted with toluene (30 mL×2), and the combined organic layers washed with brine (30 mL) and dried over Na2SO4. The solvent was removed in vacuo to yield the title compound as a as pale yellow viscous oil.

1. customA 250 mL, two-neck flask fitted with an addition funnel
2. customdid not exceed 10° C
3. additionwas added in portions over 3 minutes, while the temperature of the reaction mixture
4. temperaturewas maintained below 5° C
5. filtrationThe reaction mixture was filtered
6. customthe layers were separated
7. extractionthe aqueous layer was extracted with toluene (30 mL×2)
8. washthe combined organic layers washed with brine (30 mL)
9. dry with materialdried over Na2SO4
10. customThe solvent was removed in vacuo