反应详情

温度

175 °C

159b (0.062 g, 0.21 mmol) was ground together with P4S10 (0.047 g, 0.105 mmol) in mortar and pestle to form grey powder. The powder was stirred under argon in a flask fitted with condenser and heated to 175° C. for 2 h. The reaction flask was covered with aluminum foil during reaction. After 2 h of reaction, flask was cooled down to room temperature. 25 mL of CH2Cl2:MeOH (10%) mixtures was added and stirred for 15 min. This reaction mixture then washed with water (2×30 mL). Organic layer dried with Na2SO4 and evaporated to yield crude product which was purified by prep-TLC (Eluent —CH2Cl2:MeOH (8%) to give 162b (0.04 g, 60%) as olive green solid. 1H NMR (400 MHz, CDCl3) δ 8.47 (s, 1H), 7.82 (m, 3H), 7.50 (d, J=6.5 Hz, 1H), 7.43 (t, J=7.5 Hz, 2H), 7.34 (t, J=7.4 Hz, 1H), 6.97 (m, 1H), 6.66 (m, 1H), 4.62 (t, J=6.9 Hz, 2H), 4.48 (m, 2H). 13C NMR (100 MHz, CDCl3) δ 168.59, 155.22, 148.03, 131.85, 130.17, 128.84, 128.29, 125.61, 119.84, 113.87, 112.28, 54.99, 46.95, 28.02. HRMS (EI) calcd for C16H16N4OS [M]+ 312.104. found 312.1060.

1. customto form grey powder
2. customfitted with condenser
3. customAfter 2 h of reaction, flask
4. temperaturewas cooled down to room temperature
5. stirringstirred for 15 min
6. washThis reaction mixture then washed with water (2×30 mL)
7. dry with materialOrganic layer dried with Na2SO4
8. customevaporated
9. customto yield crude product which
10. customwas purified by prep-TLC (Eluent —CH2Cl2