反应详情

温度

110 °C

Intermediate 4 (1.075 g, 3.5 mmol), morpholin-3-one (389 mg, 3.85 mmol), CuI (67 mg, 0.35 mmol), N,N′-dimethylethylene diamine (75 μl, 0.7 mmol) and K2CO3 (1.064 g, 7.7 mmol) were suspended in toluene (30 ml) under argon and heated to 110° C. for 20 h. After cooling to RT the reaction mixture was quenched by addition of 100 ml sat. aq. NH4Cl, 150 ml concentrated NH3 in water and 100 ml water and extracted three times with ethyl acetate. The organic layers were combined and washed with water and sat. aq. NaCl-solution, dried with MgSO4, filtered and evaporated to dryness. The resulting oil crystallizes upon standing and was triturated with n-heptane-MTBE (19:1).

1. temperatureAfter cooling to RT the reaction mixture
2. customwas quenched by addition of 100 ml sat. aq. NH4Cl, 150 ml concentrated NH3 in water and 100 ml water
3. extractionextracted three times with ethyl acetate
4. washwashed with water and sat. aq. NaCl-solution
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. customevaporated to dryness
8. customThe resulting oil crystallizes
9. customwas triturated with n-heptane-MTBE (19:1)