反应详情

温度

90 °C

Compound 26 (11.1 mg, 0.028 mmol) is dissolved partially in an aqueous solution of hydrochloric acid (6 M, 3.0 mL) in air and heated at 90° C. to give an amber solution. After 22 h of heating, the solvent is removed under reduced pressure. The residue is dissolved in water (˜3 mL) and titrated to pH 7 with dilute sodium hydroxide. The precipitated solid is collected by filtration, washed with water (2×10 mL), and dried in vacuo to give 27 as a yellow solid (98% purity by HPLC). mp >241-242° C. dec. 1H NMR (DMSO-d6/acetic acid-d4 (5:1 v/v)): δ 1.19 (m, 2H, c-Pr CH2), 1.29 (m, 2H, c-Pr CH2), 2.72 (m, 2H, NCH2CH2), 3.33 (m, 2H, NCH2CH2), 3.54 (m, 1H, c-Pr CH), 3.80 (m, 2H, NCH2CH), 6.21 (m, 1H, NCH2CH), 7.87 (br, 1H, aromatic), 7.91 (br, 1H, aromatic). 19F{1H} NMR (DMSO-d6/acetic acid-d4 (5:1 v/v)): δ −121.4 (s). LCMS m/z calcd for C18H16FN3O2S ([M]+) 357. Found 358 ([M+H]+). HRMS m/z calcd for C18H16FN3NaO2S ([M+Na]+) 380.0845. Found 380.0847.

1. customto give an amber solution
2. temperatureAfter 22 h of heating
3. customthe solvent is removed under reduced pressure
4. dissolutionThe residue is dissolved in water (˜3 mL)
5. filtrationThe precipitated solid is collected by filtration
6. washwashed with water (2×10 mL)
7. customdried in vacuo