Technology Process of rac-6-(2-fluorophenyl)-8-iodo-4-methoxy-1-methyl-4H-<1,2,4>triazolo<4,3-a><1,4>benzodiazepine
There total 8 articles about rac-6-(2-fluorophenyl)-8-iodo-4-methoxy-1-methyl-4H-<1,2,4>triazolo<4,3-a><1,4>benzodiazepine which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
thionyl chloride; triethylamine;
In
methanol; dichloromethane;
- Guidance literature:
-
Multi-step reaction with 8 steps
1: liquid ammonia / CH2Cl2 / 16 h / Heating
2: HOAc / ethanol / 0.5 h / Heating
3: 80 percent / P2S5, NaHCO3 / bis-(2-methoxy-ethyl) ether / 3 h / 80 - 85 °C
4: 83 percent / hydrazine / propan-2-ol; tetrahydrofuran / 0.25 h / Ambient temperature
5: 92 percent / silica gel / toluene / 3 h / Heating
6: 1.) t-BuOK, triethyl phosphite, 2.) O2 / 1.) THF, t-BuOH, DMF, from -20 to -10 deg C, 1 h
7: SOCl2 / CH2Cl2 / 2 h / Ambient temperature
8: Et3N / 0.08 h / Heating
With
thionyl chloride; tetraphosphorus decasulfide; potassium tert-butylate; ammonia; oxygen; silica gel; sodium hydrogencarbonate; acetic acid; triethylamine; hydrazine; triethyl phosphite;
In
tetrahydrofuran; ethanol; dichloromethane; diethylene glycol dimethyl ether; isopropyl alcohol; toluene;
DOI:10.1021/jm00107a048
- Guidance literature:
-
Multi-step reaction with 10 steps
1: iodine monochloride / CH2Cl2 / 5 h / -60 °C
2: 10percent aq. Na2CO3 / CH2Cl2 / 0.5 h / 0 °C
3: liquid ammonia / CH2Cl2 / 16 h / Heating
4: HOAc / ethanol / 0.5 h / Heating
5: 80 percent / P2S5, NaHCO3 / bis-(2-methoxy-ethyl) ether / 3 h / 80 - 85 °C
6: 83 percent / hydrazine / propan-2-ol; tetrahydrofuran / 0.25 h / Ambient temperature
7: 92 percent / silica gel / toluene / 3 h / Heating
8: 1.) t-BuOK, triethyl phosphite, 2.) O2 / 1.) THF, t-BuOH, DMF, from -20 to -10 deg C, 1 h
9: SOCl2 / CH2Cl2 / 2 h / Ambient temperature
10: Et3N / 0.08 h / Heating
With
thionyl chloride; tetraphosphorus decasulfide; potassium tert-butylate; ammonia; oxygen; silica gel; Iodine monochloride; sodium hydrogencarbonate; sodium carbonate; acetic acid; triethylamine; hydrazine; triethyl phosphite;
In
tetrahydrofuran; ethanol; dichloromethane; diethylene glycol dimethyl ether; isopropyl alcohol; toluene;
DOI:10.1021/jm00107a048