Phosphorus oxide (P4O10) → 5,6-Dimethyl-8-propyl-1-thia-3,4,7,8a-tetraaza-as-indacene
反応式
[CH3:1][C:2]1[N:3]=[C:4]([CH2:16][CH2:17][CH3:18])[N:5]([C:7]2[S:11][CH:10]=[N:9][C:8]=2[NH:12][C:13](=O)[CH3:14])[CH:6]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O=P(Cl)(Cl)Cl>>[CH3:14][C:13]1[C:6]2[N:5]([C:4]([CH2:16][CH2:17][CH3:18])=[N:3][C:2]=2[CH3:1])[C:7]2[S:11][CH:10]=[N:9][C:8]=2[N:12]=1参加物
4
反応条件
- 温度
- 110 °C
実験手順
N-(5-(4-methyl-2-propyl-1H-imidazol-1-yl)thiazol-4-yl)acetamide from example 2.5 (8 mg, 0.030 mmol) and phosphorus pentoxide (21.48 mg, 0.15 mmol) were added sequentially quickly to POCl3 (5 mL). The mixture was heated to 110° C. for 4 h, POCl3 was evaporated and the residue was quenched with ice-water. The mixture was neutralized with saturated Na2CO3 solution and extracted with EA (3×20 mL). The combined organic layer was washed with brine and concentrated to give brown liquid. It was purified by pre-HPLC to give the title compound (5.0 mg, 0.02 mmol, 67.1%) as a white solid.