Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: potassium hydroxide; potassium carbonate; tetraethylammonium bromide / water / 1.33 h / 65 - 75 °C
2.1: hydrogenchloride / methanol; water / 2 h / 75 °C / |Inert atmosphere
3.1: sodium nitrite / water / 1.25 h / 0 - 5 °C / |Inert atmosphere
3.2: 1 h / 0 - 65 °C
3.3: 1 h / 40 - 50 °C
4.1: sodium acetate / acetonitrile / 0.5 h / 20 °C
4.2: 1 h / 0 - 5 °C
5.1: acetic acid / toluene / 1 h / |Reflux
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: chlorine
2.1: hydrogenchloride / methanol; water / 2 h / 75 °C / |Inert atmosphere
3.1: sodium nitrite / water / 1.25 h / 0 - 5 °C / |Inert atmosphere
3.2: 1 h / 0 - 65 °C
3.3: 1 h / 40 - 50 °C
4.1: sodium acetate / methanol / 1.33 h / -10 - 0 °C
5.1: acetic acid / ethyl acetate / 4 h / 65 - 70 °C
6.1: potassium hydroxide; potassium carbonate / water; acetone / 0.5 h / 60 - 65 °C
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: sodium methylate; bromine / methanol / 0.5 h / 0 - 5 °C
1.2: 55 - 60 °C
2.1: hydrogenchloride / toluene / 3 h / 10 - 20 °C / |Inert atmosphere
3.1: sodium acetate / acetonitrile / 0.5 h / 20 °C
3.2: 1 h / 0 - 5 °C
4.1: acetic acid / toluene / 1 h / |Reflux
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: manganese(IV) oxide; water / 120 - 135 °C / |Inert atmosphere
2.1: sodium methylate; bromine / methanol / 0.5 h / 0 - 5 °C
2.2: 55 - 60 °C
3.1: hydrogenchloride / toluene / 3 h / 10 - 20 °C / |Inert atmosphere
4.1: sodium acetate / acetonitrile / 0.5 h / 20 °C
4.2: 1 h / 0 - 5 °C
5.1: acetic acid / toluene / 1 h / |Reflux
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: hydrogenchloride / toluene / 3 h / 10 - 20 °C / |Inert atmosphere
2.1: sodium acetate / acetonitrile / 0.5 h / 20 °C
2.2: 1 h / 0 - 5 °C
3.1: acetic acid / toluene / 1 h / |Reflux
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: sodium nitrite / water / 1.25 h / 0 - 5 °C / |Inert atmosphere
1.2: 1 h / 0 - 65 °C
1.3: 1 h / 40 - 50 °C
2.1: sodium acetate / acetonitrile / 0.5 h / 20 °C
2.2: 1 h / 0 - 5 °C
3.1: acetic acid / toluene / 1 h / |Reflux
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: sodium nitrite / water / 1.25 h / 0 - 5 °C / |Inert atmosphere
1.2: 1 h / 0 - 65 °C
1.3: 1 h / 40 - 50 °C
2.1: sodium acetate / methanol / 1.33 h / -10 - 0 °C
3.1: acetic acid / ethyl acetate / 4 h / 65 - 70 °C
4.1: potassium hydroxide; potassium carbonate / water; acetone / 0.5 h / 60 - 65 °C
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
1.1: sodium acetate / acetonitrile / 0.5 h / 20 °C
1.2: 1 h / 0 - 5 °C
2.1: acetic acid / toluene / 1 h / |Reflux
View Scheme
参考文献
Shapiro, Rafael; DiCosimo, Robert; Hennessey, Susan M.; Stieglitz, Barry; Campopiano, Onorato; Chiang, George C.
Organic Process Research and Development, 2001 , vol. 5, # 6 p. 593 - 598
