HCID 86680886、化合物 → HCID 52945927、化合物
反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([NH:12][C:13]2[CH:18]=[C:17]([N+:19]([O-:21])=[O:20])[CH:16]=[CH:15][C:14]=2[OH:22])=S)=[CH:5][CH:4]=1)[CH3:2]>C(#N)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]2[O:22][C:14]3[CH:15]=[CH:16][C:17]([N+:19]([O-:21])=[O:20])=[CH:18][C:13]=3[N:12]=2)=[CH:5][CH:4]=1)[CH3:2]参加物
3
実験手順
In an ice bath under nitrogen gas, 15 mL of acetonitrile was slowly added to KO2 (12.05 mmol, 5 eq) with stirring. Then, the compound (a) synthesized in Example 1 (2.41 mmol, 1 eq) in 20 mL of acetonitrile was slowly added to said solution containing KO2. The mixture was reacted at room temperature for 16 hours, and then the reaction solution was diluted with 30 mL of ice water. This solution was extracted with dichloromethane, and washed two times with saturated aqueous NaCl solution. After drying with anhydrous MgSO4, the precipitate obtained by removing the solvent under reduced pressure was filtered under reduced pressure with EtOAc:hexane=1:10 (V/V) to yield the title compound (b). Yellow powder (88%), mp 172-173° C.; 1H NMR (Acetone-d6, 400 MHz) δ 9.805 (s, 1H), 8.229 (s, 1H), 8.109 (d, J=8.8 Hz, 1H), 7.764 (d, J=8.4 Hz, 2H), 7.615 (d, J=9.2 Hz, 1H), 7.278 (d, J=8.8 Hz, 2H), 2.651 (q, J=7.6 Hz, 2H), 1.230 (t, J=7.6 Hz, 3H).