2,4-二氯-6-(苯基甲基)-苯丙醛合成路线 （共 8 条）
反应条件
1: pyridine / 0.5 h / 0 °C
2: methanol / 1.) 20 deg C, 30 min, 2.) reflux, 1 h
3: conc. H2SO4 / acetone; H2O / 16 h / Heating
4: diethyl ether / 1.5 h / 0 - 20 °C
5: trifluoroacetic anhydride, Me2SO / CH2Cl2 / 0.5 h / -78 °C
6: 55 percent / hydrazine, KOH / bis-(2-hydroxy-ethyl) ether / 15 h / 200 - 205 °C
7: 1.) N-chlorosuccinimide, 2.) CuBr2, CuO / 1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min
View Scheme
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
反应条件
1: diethyl ether / 1.5 h / 0 - 20 °C
2: trifluoroacetic anhydride, Me2SO / CH2Cl2 / 0.5 h / -78 °C
3: 55 percent / hydrazine, KOH / bis-(2-hydroxy-ethyl) ether / 15 h / 200 - 205 °C
4: 1.) N-chlorosuccinimide, 2.) CuBr2, CuO / 1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min
View Scheme
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
反应条件
1: 88 percent / lithium aluminum hydride / diethyl ether / 1.) 20 deg C, 0.5 h, 2.) reflux, 1 h
2: pyridine / 0.5 h / 0 °C
3: methanol / 1.) 20 deg C, 30 min, 2.) reflux, 1 h
4: conc. H2SO4 / acetone; H2O / 16 h / Heating
5: diethyl ether / 1.5 h / 0 - 20 °C
6: trifluoroacetic anhydride, Me2SO / CH2Cl2 / 0.5 h / -78 °C
7: 55 percent / hydrazine, KOH / bis-(2-hydroxy-ethyl) ether / 15 h / 200 - 205 °C
8: 1.) N-chlorosuccinimide, 2.) CuBr2, CuO / 1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min
View Scheme
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
反应条件
1: 55 percent / hydrazine, KOH / bis-(2-hydroxy-ethyl) ether / 15 h / 200 - 205 °C
2: 1.) N-chlorosuccinimide, 2.) CuBr2, CuO / 1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min
View Scheme
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
反应条件
1: trifluoroacetic anhydride, Me2SO / CH2Cl2 / 0.5 h / -78 °C
2: 55 percent / hydrazine, KOH / bis-(2-hydroxy-ethyl) ether / 15 h / 200 - 205 °C
3: 1.) N-chlorosuccinimide, 2.) CuBr2, CuO / 1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min
View Scheme
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
反应条件
1: methanol / 1.) 20 deg C, 30 min, 2.) reflux, 1 h
2: conc. H2SO4 / acetone; H2O / 16 h / Heating
3: diethyl ether / 1.5 h / 0 - 20 °C
4: trifluoroacetic anhydride, Me2SO / CH2Cl2 / 0.5 h / -78 °C
5: 55 percent / hydrazine, KOH / bis-(2-hydroxy-ethyl) ether / 15 h / 200 - 205 °C
6: 1.) N-chlorosuccinimide, 2.) CuBr2, CuO / 1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min
View Scheme
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
反应条件
1: diethyl ether / 1.5 h / 0 - 20 °C
2: trifluoroacetic anhydride, Me2SO / CH2Cl2 / 0.5 h / -78 °C
3: 55 percent / hydrazine, KOH / bis-(2-hydroxy-ethyl) ether / 15 h / 200 - 205 °C
4: 1.) N-chlorosuccinimide, 2.) CuBr2, CuO / 1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min
View Scheme
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
反应条件
N-chloro-succinimide; copper(II) oxide; copper(ll) bromide
1.) CCl4, 0 deg C, 4 h, 2.) THF, H2O, reflux, 10 min; Yield given. Multistep reaction;
参考文献
Stokker, G. E.; Alberts, A. W.; Anderson, P. S.; Cragoe, E. J.; Deana, A. A.; et al.
Journal of Medicinal Chemistry, 1986 , vol. 29, # 2 p. 170 - 181
