7-溴-2,3-二氢-1H-1-苯氮杂卓-4-羧酸甲酯合成路线 （共 7 条）
反应条件
hydrogenchloride in ethyl acetate T=80°C; 0.5 h;
参考文献
Seto, Masaki; Aramaki, Yoshio; Okawa, Tomohiro; Miyamoto, Naoki; Aikawa, Katsuji; Kanzaki, Naoyuki; Niwa, Shin-Ichi; Iizawa, Yuji; Baba, Masanori; Shiraishi, Mitsuru
Chemical and Pharmaceutical Bulletin, 2004 , vol. 52, # 5 p. 577 - 590
反应条件
1: NaBH4 / tetrahydrofuran; methanol / 1 h / -15 °C 2: Et3N / tetrahydrofuran / 14 h / 20 °C 3: 2.53 g / 1,8-diazabicyclo[5,4,0]undec-7-ene / tetrahydrofuran / 0.17 h / Heating 4: 100 percent / aq. HCl / ethyl acetate / 0.5 h / 80 °C View Scheme
参考文献
Takeda Chemical Industries, Ltd.
Patent: EP1186604 A1, 2002 ;
EP 1186604 A1
反应条件
1: DMAP / tetrahydrofuran / 1.5 h / Heating 2: 3.89 g / sodium methoxide / 2.5 h / Heating 3: NaBH4 / tetrahydrofuran; methanol / 1 h / -15 °C 4: Et3N / tetrahydrofuran / 14 h / 20 °C 5: 2.53 g / 1,8-diazabicyclo[5,4,0]undec-7-ene / tetrahydrofuran / 0.17 h / Heating 6: 100 percent / aq. HCl / ethyl acetate / 0.5 h / 80 °C View Scheme
参考文献
Seto, Masaki; Aramaki, Yoshio; Okawa, Tomohiro; Miyamoto, Naoki; Aikawa, Katsuji; Kanzaki, Naoyuki; Niwa, Shin-Ichi; Iizawa, Yuji; Baba, Masanori; Shiraishi, Mitsuru
Chemical and Pharmaceutical Bulletin, 2004 , vol. 52, # 5 p. 577 - 590
反应条件
1.1: NaH / dimethylformamide / 1 h / 20 °C 1.2: NaI / dimethylformamide / 14 h / 80 °C 2.1: 25.1 g / NaH / dimethylformamide / 15 h / 80 °C 3.1: 21 percent / H2SO4; AcOH / 2.5 h / 90 °C 4.1: DMAP / tetrahydrofuran / 1.5 h / Heating 5.1: 3.89 g / sodium methoxide / 2.5 h / Heating 6.1: NaBH4 / tetrahydrofuran; methanol / 1 h / -15 °C 7.1: Et3N / tetrahydrofuran / 14 h / 20 °C 8.1: 2.53 g / 1,8-diazabicyclo[5,4,0]undec-7-ene / tetrahydrofuran / 0.17 h / Heating 9.1: 100 percent / aq. HCl / ethyl acetate / 0.5 h / 80 °C View Scheme
参考文献
Seto, Masaki; Aramaki, Yoshio; Okawa, Tomohiro; Miyamoto, Naoki; Aikawa, Katsuji; Kanzaki, Naoyuki; Niwa, Shin-Ichi; Iizawa, Yuji; Baba, Masanori; Shiraishi, Mitsuru
Chemical and Pharmaceutical Bulletin, 2004 , vol. 52, # 5 p. 577 - 590
反应条件
1.1: 88 percent / pyridine / 1 h / 55 °C 2.1: NaH / dimethylformamide / 1 h / 20 °C 2.2: NaI / dimethylformamide / 14 h / 80 °C 3.1: 25.1 g / NaH / dimethylformamide / 15 h / 80 °C 4.1: 21 percent / H2SO4; AcOH / 2.5 h / 90 °C 5.1: DMAP / tetrahydrofuran / 1.5 h / Heating 6.1: 3.89 g / sodium methoxide / 2.5 h / Heating 7.1: NaBH4 / tetrahydrofuran; methanol / 1 h / -15 °C 8.1: Et3N / tetrahydrofuran / 14 h / 20 °C 9.1: 2.53 g / 1,8-diazabicyclo[5,4,0]undec-7-ene / tetrahydrofuran / 0.17 h / Heating 10.1: 100 percent / aq. HCl / ethyl acetate / 0.5 h / 80 °C View Scheme
参考文献
Seto, Masaki; Aramaki, Yoshio; Okawa, Tomohiro; Miyamoto, Naoki; Aikawa, Katsuji; Kanzaki, Naoyuki; Niwa, Shin-Ichi; Iizawa, Yuji; Baba, Masanori; Shiraishi, Mitsuru
Chemical and Pharmaceutical Bulletin, 2004 , vol. 52, # 5 p. 577 - 590
反应条件
1: 3.89 g / sodium methoxide / 2.5 h / Heating 2: NaBH4 / tetrahydrofuran; methanol / 1 h / -15 °C 3: Et3N / tetrahydrofuran / 14 h / 20 °C 4: 2.53 g / 1,8-diazabicyclo[5,4,0]undec-7-ene / tetrahydrofuran / 0.17 h / Heating 5: 100 percent / aq. HCl / ethyl acetate / 0.5 h / 80 °C View Scheme
参考文献
Seto, Masaki; Aramaki, Yoshio; Okawa, Tomohiro; Miyamoto, Naoki; Aikawa, Katsuji; Kanzaki, Naoyuki; Niwa, Shin-Ichi; Iizawa, Yuji; Baba, Masanori; Shiraishi, Mitsuru
Chemical and Pharmaceutical Bulletin, 2004 , vol. 52, # 5 p. 577 - 590
反应条件
sulfuric acid T=0 - 80°C; 10 h;
参考文献
Takeda Chemical Industries, Ltd.
Patent: EP1186604 A1, 2002 ;
Location in patent: Page 115 ;
EP 1186604 A1
