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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
磷酸西他列汀一水合物
合成路线
(共 9 条)
486460-32-6
西他列汀
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
phosphoric acid; water in isopropyl alcohol T=20 - 75°C;
参考文献
Lin, Kuaile; Cai, Zhengyan; Zhou, Weicheng
Synthetic Communications, 2013 , vol. 43, # 24 p. 3281 - 3286
764667-65-4
(2Z)-4-氧代-4-[3-(三氟甲基)-5,6-二氢-[1,2,4]三唑并[4,3-a]吡嗪-7-(8H)-基]-1-(2,4,5-三氟苯基)丁-2-酮
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1: isopropyl alcohol; acetic acid / 18 h / 50 °C 2: sodium tetrahydroborate; formic acid / tetrahydrofuran / -30 °C 3: 20 palladium(II) hydroxide on carbon; hydrogen; acetic acid / methanol; water / 14 h / 50 °C / 7500.75 Torr 4: phosphoric acid; water / isopropyl alcohol / 20 - 75 °C View Scheme
参考文献
Synthetic Communications, , vol. 43, # 24 p. 3281 - 3286
1169707-29-2
(2Z)-1-[5,6-二氢-3-(三氟甲基)-1,2,4-三唑并[4,3-a]吡嗪-7(8H)-基]-3-[[(1R)-1-苯乙基]氨基]-4-(2,4,5-三氟苯基)-2-丁烯-1-酮
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1: sodium tetrahydroborate; formic acid / tetrahydrofuran / -30 °C 2: 20 palladium(II) hydroxide on carbon; hydrogen; acetic acid / methanol; water / 14 h / 50 °C / 7500.75 Torr 3: phosphoric acid; water / isopropyl alcohol / 20 - 75 °C View Scheme
参考文献
Synthetic Communications, , vol. 43, # 24 p. 3281 - 3286
1169707-30-5
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1: 20 palladium(II) hydroxide on carbon; hydrogen; acetic acid / methanol; water / 14 h / 50 °C / 7500.75 Torr 2: phosphoric acid; water / isopropyl alcohol / 20 - 75 °C View Scheme
参考文献
Synthetic Communications, , vol. 43, # 24 p. 3281 - 3286
868071-17-4
(3S)-2’,4’,5’-三氟-3-羟基苯丁酸
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1.1: lithium hydroxide hydrate; dicyclohexyl-carbodiimide / tetrahydrofuran; water; cis-1,2-dichloroethylene / 3 h / 20 - 22 °C 1.2: 18.5 h / 10 - 20 °C 2.1: lithium hydroxide hydrate / tetrahydrofuran; water / 2.33 h / 20 - 25 °C / pH 3 2.2: 3 h / 0 - 5 °C 3.1: phosphoric acid / isopropyl alcohol / 16 h / 30 °C 4.1: sodium hydroxide / water / 1 h / 0 - 5 °C 5.1: phosphoric acid; water / water; isopropyl alcohol / 0.25 h View Scheme
参考文献
US2013/158265 A1, ;
767352-30-7
(4R)-1-苯甲氧基-4-[(2,4,5-三氟苯基)甲基]-2-氮杂环丁酮
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1.1: lithium hydroxide hydrate / tetrahydrofuran; water / 2.33 h / 20 - 25 °C / pH 3 1.2: 3 h / 0 - 5 °C 2.1: phosphoric acid / isopropyl alcohol / 16 h / 30 °C 3.1: sodium hydroxide / water / 1 h / 0 - 5 °C 4.1: phosphoric acid; water / water; isopropyl alcohol / 0.25 h View Scheme
参考文献
US2013/158265 A1, ;
1361389-75-4
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1: phosphoric acid / isopropyl alcohol / 16 h / 30 °C 2: sodium hydroxide / water / 1 h / 0 - 5 °C 3: phosphoric acid; water / water; isopropyl alcohol / 0.25 h View Scheme
参考文献
US2013/158265 A1, ;
769195-26-8
3-氧代-4-(2,4,5-三氟苯基)丁酸甲酯
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1.1: hydrogen; dichloro[(S)-(-)-2,2'-bis(diphenylphosphino)-1,1'-binaphthyl]ruthenium(II) / methanol; acetic acid / 70 °C / 3620.13 Torr / |Inert atmosphere; |Autoclave 2.1: lithium hydroxide hydrate; dicyclohexyl-carbodiimide / tetrahydrofuran; water; cis-1,2-dichloroethylene / 3 h / 20 - 22 °C 2.2: 18.5 h / 10 - 20 °C 3.1: lithium hydroxide hydrate / tetrahydrofuran; water / 2.33 h / 20 - 25 °C / pH 3 3.2: 3 h / 0 - 5 °C 4.1: phosphoric acid / isopropyl alcohol / 16 h / 30 °C 5.1: sodium hydroxide / water / 1 h / 0 - 5 °C 6.1: phosphoric acid; water / water; isopropyl alcohol / 0.25 h View Scheme
参考文献
US2013/158265 A1, ;
209995-38-0
2,4,5-三氟苯乙酸
→
反应条件
654671-77-9
磷酸西他列汀一水合物
反应条件
1.1: triethylamine; magnesium chloride / acetonitrile / 30 - 50 °C / |Inert atmosphere 1.2: 5.5 h / 30 °C / |Inert atmosphere 2.1: hydrogen; dichloro[(S)-(-)-2,2'-bis(diphenylphosphino)-1,1'-binaphthyl]ruthenium(II) / methanol; acetic acid / 70 °C / 3620.13 Torr / |Inert atmosphere; |Autoclave 3.1: lithium hydroxide hydrate; dicyclohexyl-carbodiimide / tetrahydrofuran; water; cis-1,2-dichloroethylene / 3 h / 20 - 22 °C 3.2: 18.5 h / 10 - 20 °C 4.1: lithium hydroxide hydrate / tetrahydrofuran; water / 2.33 h / 20 - 25 °C / pH 3 4.2: 3 h / 0 - 5 °C 5.1: phosphoric acid / isopropyl alcohol / 16 h / 30 °C 6.1: sodium hydroxide / water / 1 h / 0 - 5 °C 7.1: phosphoric acid; water / water; isopropyl alcohol / 0.25 h View Scheme
参考文献
US2013/158265 A1, ;