反应详情

温度

105 °C

To a suspension of Compound 239 (150 mg, 0.38 mmol) in pyridine (2.0 mL) was added 3-(dimethylamino)propanoyl chloride (71 mg, 0.38 mmol) and the reaction mixture was heated at 105° C. for 5 h. and quenched with aqueous NH4Cl solution. Organic matter was extracted with CH2Cl2 (with 10% EtOH) and washed with brine. The organic extracts were dried (Na2SO4) and concentrated and purified by preparative HPLC to yield the title compound (103 mg, 55%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.16 (t, J=7.33 Hz, 3 H) 2.24 (s, 3 H) 2.33 (s, 6 H) 2.56 (t, J=5.81 Hz, 2 H) 2.62 (t, J=5.31 Hz, 2 H) 3.41 (d, J=7.33 Hz, 2 H) 3.93 (s, 3 H) 7.41 (d, J=1.26 Hz, 1 H) 7.87 (t, J=7.71 Hz, 1 H) 7.93-7.97 (m, 1 H) 8.03 (d, J=8.84 Hz, 1 H) 8.06 (s, 2 H) 8.22 (d, J=2.02 Hz, 1 H) 10.99 (br. s., 1 H) 12.07 (s, 1 H); [M+H] calc'd for C26H31N4O—4S, 495.2; found, 495.4.

1. customquenched with aqueous NH4Cl solution
2. extractionOrganic matter was extracted with CH2Cl2 (with 10% EtOH)
3. washwashed with brine
4. dry with materialThe organic extracts were dried (Na2SO4)
5. concentrationconcentrated
6. custompurified by preparative HPLC