Technology Process of cyclohex-3-ene-1-carboxylic acid (R)-(+)-1-phenylethanamine salt
There total 1 articles about cyclohex-3-ene-1-carboxylic acid (R)-(+)-1-phenylethanamine salt which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
acetone;
at 55 - 60 ℃;
for 2.83333h;
Reflux;
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: acetone / 0.25 h / Reflux; Resolution of racemate
2.1: hydrogenchloride / water; tert-butyl methyl ether / 0.25 h / 20 - 25 °C
3.1: triethylamine; diphenyl phosphoryl azide / toluene; tert-butyl alcohol / 0.25 h / 20 - 60 °C
3.2: 0.83 h / 50 °C
4.1: 3-chloro-benzenecarboperoxoic acid / dichloromethane / 0.5 h / 30 - 40 °C / Cooling with ice
5.1: toluene / 15 - 25 °C
5.2: 30 °C
5.3: 40 - 45 °C
6.1: hydrazine hydrate; diothiothreitol / dichloromethane / 0.42 h / 15 - 25 °C / Inert atmosphere
6.2: 0.48 h
7.1: sodium hydroxide / benzyltri(n-butyl)ammonium chloride / water; tert-butyl methyl ether / 0.08 h / 20 - 25 °C / Inert atmosphere
With
hydrogenchloride; diphenyl phosphoryl azide; hydrazine hydrate; triethylamine; 3-chloro-benzenecarboperoxoic acid; sodium hydroxide; diothiothreitol;
benzyltri(n-butyl)ammonium chloride;
In
dichloromethane; tert-butyl methyl ether; water; acetone; toluene; tert-butyl alcohol;
3.1: Curtius Rearrangement;
- Guidance literature:
-
Multi-step reaction with 8 steps
1.1: acetone / 0.25 h / Reflux; Resolution of racemate
2.1: hydrogenchloride / water; tert-butyl methyl ether / 0.25 h / 20 - 25 °C
3.1: triethylamine; diphenyl phosphoryl azide / toluene; tert-butyl alcohol / 0.25 h / 20 - 60 °C
3.2: 0.83 h / 50 °C
4.1: 3-chloro-benzenecarboperoxoic acid / dichloromethane / 0.5 h / 30 - 40 °C / Cooling with ice
5.1: toluene / 15 - 25 °C
5.2: 30 °C
5.3: 40 - 45 °C
6.1: hydrazine hydrate; diothiothreitol / dichloromethane / 0.42 h / 15 - 25 °C / Inert atmosphere
6.2: 0.48 h
7.1: sodium hydroxide / benzyltri(n-butyl)ammonium chloride / water; tert-butyl methyl ether / 0.08 h / 20 - 25 °C / Inert atmosphere
8.1: phosphoric acid / isopropyl alcohol / 35 - 50 °C
With
hydrogenchloride; phosphoric acid; diphenyl phosphoryl azide; hydrazine hydrate; triethylamine; 3-chloro-benzenecarboperoxoic acid; sodium hydroxide; diothiothreitol;
benzyltri(n-butyl)ammonium chloride;
In
dichloromethane; tert-butyl methyl ether; water; isopropyl alcohol; acetone; toluene; tert-butyl alcohol;
3.1: Curtius Rearrangement;