2749-59-9

基本信息
1,3-二甲基吡唑-5-酮
1,3-二甲基-5-氧代吡唑啉
1,3-二甲基-5-吡唑啉酮
1,3-DIMETHYL-4,5-DIHYDRO-1H-PYRAZOL-5-ONE
1,3-DIMETHYL-5-PYRAZOLONE
1,3-DIMETHYLPYRAZOLONE
2,4-DIHYDRO-2,5-DIMETHYL-3H-PYRAZOL-3-ONE
BUTTPARK 82\11-61
1,3-Dimethyl-5-pyrazolinone
2,5-Dimethyl-2,4-dihydro-3H-pyrazol-3-one
2-Pyrazolin-5-one, 1,3-dimethyl-
1,3-dimethyl-5-pyrazolone(DMP)
3H-PYRAZOL-3-ONE, 2,4-DIHYDRO-2,5-DIMETHYL-
1,3-dimethyl-1H-pyrazol-5(4H)-one
1,3-DIMETHYL-5-PYRAZOLONE 95+%
2,5-Dimethyl-2,4-dihydro-3H-pyrazole-3-one
2,5-Dimethyl-2H-pyrazole-3(4H)-one
物理化學性質(zhì)
安全數(shù)據(jù)
制備方法

141-97-9

60-34-4

2749-59-9
在0℃條件下,向3-氧代己酸乙酯(11.06g,84.99mmol)的無水乙醇(100mL)溶液中緩慢滴加甲基肼(4.47mL,84.99mmol)。反應體系自然升溫至室溫,持續(xù)攪拌3.5小時。隨后,將反應混合物加熱至60℃,繼續(xù)反應10小時,并保持回流狀態(tài)2.5小時。反應完成后,使用旋轉(zhuǎn)蒸發(fā)儀將混合物濃縮至干,得到中間體4,為粘稠的粉紅色固體(9.52g,收率100%)。中間體4的結(jié)構(gòu)通過1H NMR(400MHz,CDCl3)和質(zhì)譜(ESI)進行確認:1H NMR(400MHz,CDCl3)δ(ppm):5.06(s,1H),3.85(bs,1H),3.32(s,3H),1.94(s,3H);MS(ESI):m/z計算值(C15H9N2O)為113.1,實測值為113.2([M+H]+)。
參考文獻:
[1] Bioorganic and Medicinal Chemistry Letters, 2005, vol. 15, # 13, p. 3307 - 3312
[2] Patent: WO2016/205460, 2016, A1. Location in patent: Paragraph 0140-0141
[3] Patent: WO2016/7905, 2016, A1. Location in patent: Page/Page column 37
[4] Bioorganic and Medicinal Chemistry Letters, 2016, vol. 26, # 23, p. 5815 - 5818
[5] Patent: US4382948, 1983, A