反应详情

Cyclopropylmethyl amine (0.30 mL, 3.34 mmol) was added to a solution of Example 102j (0.2 g, 0.42 mmol) in methanol (5 mL), followed by the addition of n-tetrabutylammonium iodide (0.01 g, 0.020 mmol) in an atmosphere of nitrogen and sealed in a pressure reactor vessel at 110° C. for 10 h. The reaction mixture was brought to room temperature, concentrated, treated with water and extracted with n-butanol. The organic layer was washed with water, brine, dried, concentrated and purified by crystallisation (ethylacetate-pet-ether). Yield: 0.114 g, (53.7%). 1H NMR (DMSO-d6): δ 0.1 (d, 2H, CH2), 0.50 (d, 2H, CH2), 0.90 (m, 1H, CH), 2.30 (d, 2H, CH2), 2.70 (s, 3H, CH3), 3.20-3.25 (m, 4H, 2CH2), 5.15 (s, 2H, CH2), 7.10 (s, 1H, Ar), 7.15 (s, 1H, Ar), 8.0 (s, 1H, Ar), 8.20 (s, 1H, Ar).

1. customsealed in a pressure reactor vessel at 110° C. for 10 h
2. customwas brought to room temperature
3. concentrationconcentrated
4. additiontreated with water
5. extractionextracted with n-butanol
6. washThe organic layer was washed with water, brine
7. customdried
8. concentrationconcentrated
9. custompurified by crystallisation (ethylacetate-pet-ether)