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结构式
乙二醇
甲醛
63148-62-9
MDI
丁酮
二甲基亚砜
碳酸氢钠
471-34-1
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乙二醇
甲醛
63148-62-9
MDI
丁酮
二甲基亚砜
碳酸氢钠
471-34-1
143150-92-9
合成路线
(共 8 条)
17899-48-8
5-甲基-4,5,6,7-四氢[1,3]噻唑并[5,4-C]吡啶-2-胺
→
反应条件
143150-92-9
反应条件
hydrogen bromide; sodium nitrite in water T=0 - 30°C; 25.5 h;
参考文献
DAIICHI SANKYO COMPANY, LIMITED; Kawanami, Koutarou
Patent: US2013/144061 A1, 2013 ;
Location in patent: Paragraph 0248; 0249; 0250 ;
50-00-0
甲醛
→
反应条件
143150-92-9
反应条件
sodium tris(acetoxy)borohydride; acetic acid; triethylamine in dichloromethane; water T=20°C; 1 h;
参考文献
DAIICHI PHARMACEUTICAL CO., LTD.
Patent: EP1405852 A1, 2004 ;
Location in patent: Page 66 ;
EP 1405852 A1
→
反应条件
143150-92-9
反应条件
sodium hydroxide; formaldehyd; sodium tris(acetoxy)borohydride; acetic acid; triethylamine in dichloromethane
参考文献
DAIICHI PHARMACEUTICAL CO., LTD.
Patent: US2005/20645 A1, 2005 ;
50-00-0
甲醛
+
365996-07-2
2-溴-4,5,6,7-四氢噻唑并[5,4-c]吡啶盐酸盐
→
反应条件
143150-92-9
反应条件
sodium tris(acetoxy)borohydride; acetic acid; triethylamine in diethyl ether; dichloromethane; water T=20°C; 1 h;
参考文献
Haginoya, Noriyasu; Komoriya, Satoshi; Osanai, Ken; Yoshino, Toshiharu; Nagata, Tsutomu; Nagamochi, Masatoshi; Muto, Ryo; Yamaguchi, Mitsuhiro; Nagahara, Takayasu; Kanno, Hideyuki
Heterocycles, 2004 , vol. 63, # 7 p. 1555 - 1561
79099-07-3
N-叔丁氧羰基-4-哌啶酮
→
反应条件
143150-92-9
反应条件
1.1: pyrrolidine; TsOH*H2O / cyclohexane / 2 h / Heating 1.2: 63 percent / S8 / methanol / 5 h / 0 °C 2.1: 49 percent / t-BuONO; CuBr2 / dimethylformamide / 2 h / 50 - 60 °C 3.1: TFA / CH2Cl2 / 0.17 h / 20 °C 4.1: 49.0 g / NaBH(OAc)3; Et3N; AcOH / H2O; CH2Cl2; diethyl ether / 1 h / 20 °C View Scheme
参考文献
Haginoya, Noriyasu; Komoriya, Satoshi; Osanai, Ken; Yoshino, Toshiharu; Nagata, Tsutomu; Nagamochi, Masatoshi; Muto, Ryo; Yamaguchi, Mitsuhiro; Nagahara, Takayasu; Kanno, Hideyuki
Heterocycles, 2004 , vol. 63, # 7 p. 1555 - 1561
365996-06-1
2-溴-6,7-二氢噻唑并[5,4-c]吡啶-5(4H)-羧酸叔丁酯
→
反应条件
143150-92-9
反应条件
1: TFA / CH2Cl2 / 0.17 h / 20 °C 2: 49.0 g / NaBH(OAc)3; Et3N; AcOH / H2O; CH2Cl2; diethyl ether / 1 h / 20 °C View Scheme
参考文献
Haginoya, Noriyasu; Komoriya, Satoshi; Osanai, Ken; Yoshino, Toshiharu; Nagata, Tsutomu; Nagamochi, Masatoshi; Muto, Ryo; Yamaguchi, Mitsuhiro; Nagahara, Takayasu; Kanno, Hideyuki
Heterocycles, 2004 , vol. 63, # 7 p. 1555 - 1561
365996-05-0
2-氨基-6,7-二氢噻唑并[5,4-c]吡啶-5(4H)-甲酸叔丁酯
→
反应条件
143150-92-9
反应条件
1: 49 percent / t-BuONO; CuBr2 / dimethylformamide / 2 h / 50 - 60 °C 2: TFA / CH2Cl2 / 0.17 h / 20 °C 3: 49.0 g / NaBH(OAc)3; Et3N; AcOH / H2O; CH2Cl2; diethyl ether / 1 h / 20 °C View Scheme
参考文献
Haginoya, Noriyasu; Komoriya, Satoshi; Osanai, Ken; Yoshino, Toshiharu; Nagata, Tsutomu; Nagamochi, Masatoshi; Muto, Ryo; Yamaguchi, Mitsuhiro; Nagahara, Takayasu; Kanno, Hideyuki
Heterocycles, 2004 , vol. 63, # 7 p. 1555 - 1561
1445-73-4
N-甲基-4-哌啶酮
→
反应条件
143150-92-9
反应条件
1: pyrrolidine; sulfur / isopropyl alcohol / 1 h / 50 - 64 °C 2: hydrogen bromide; sodium nitrite / water / 25.5 h / 0 - 30 °C View Scheme
参考文献
DAIICHI SANKYO COMPANY, LIMITED; Kawanami, Koutarou
Patent: US2013/144061 A1, 2013 ;