Technology Process of 2,6-Dichloro-5-fluoro-N-(2-hydroxy-1,1-dimethyl-ethyl)-nicotinamide
There total 1 articles about 2,6-Dichloro-5-fluoro-N-(2-hydroxy-1,1-dimethyl-ethyl)-nicotinamide which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
Multi-step reaction with 2 steps
1: 84 percent / SOCl2, DMF / toluene / 3 h / 85 °C
2: 96 percent / CH2Cl2 / 3 h / Ambient temperature
With
thionyl chloride; N,N-dimethyl-formamide;
In
dichloromethane; toluene;
DOI:10.1016/0968-0896(96)00106-X
- Guidance literature:
-
Multi-step reaction with 10 steps
1: 87 percent / SOCl2 / CH2Cl2 / 22.5 h / Ambient temperature
2: 1.) LDA / 1.) THF, -78 deg C, 15 min, 2.) THF, 0 deg C, 30 min
3: 66 percent / LiAlH4 / diethyl ether / 1 h / 0 °C
4: 45 percent / NaH / tetrahydrofuran / Heating
5: 10percent aq. HCl / 22 h / 90 - 95 °C
6: dioxane / 1 h / Ambient temperature
7: 100 percent / SOCl2, DMF / 2.5 h / Ambient temperature
8: 1.) LDA / 1.) -78 deg C, 2.) from -78 deg C to 0 deg C
9: Ac2O / Heating
10: CH2Cl2 / 2 h / Ambient temperature
With
hydrogenchloride; lithium aluminium tetrahydride; thionyl chloride; acetic anhydride; sodium hydride; N,N-dimethyl-formamide; lithium diisopropyl amide;
In
tetrahydrofuran; 1,4-dioxane; diethyl ether; dichloromethane;
DOI:10.1016/0968-0896(96)00106-X
- Guidance literature:
-
Multi-step reaction with 11 steps
1: 87 percent / SOCl2 / CH2Cl2 / 22.5 h / Ambient temperature
2: 1.) LDA / 1.) THF, -78 deg C, 15 min, 2.) THF, 0 deg C, 30 min
3: 66 percent / LiAlH4 / diethyl ether / 1 h / 0 °C
4: 45 percent / NaH / tetrahydrofuran / Heating
5: 10percent aq. HCl / 22 h / 90 - 95 °C
6: dioxane / 1 h / Ambient temperature
7: 100 percent / SOCl2, DMF / 2.5 h / Ambient temperature
8: 1.) LDA / 1.) -78 deg C, 2.) from -78 deg C to 0 deg C
9: Ac2O / Heating
10: CH2Cl2 / 2 h / Ambient temperature
11: 47 percent / NaH / tetrahydrofuran / 0.83 h / 45 - 50 °C
With
hydrogenchloride; lithium aluminium tetrahydride; thionyl chloride; acetic anhydride; sodium hydride; N,N-dimethyl-formamide; lithium diisopropyl amide;
In
tetrahydrofuran; 1,4-dioxane; diethyl ether; dichloromethane;
DOI:10.1016/0968-0896(96)00106-X