1-Hydroxyethylethoxypiperazine synthesis
- Product Name:1-Hydroxyethylethoxypiperazine
- CAS Number:13349-82-1
- Molecular formula:C8H18N2O2
- Molecular Weight:174.24
166388-52-9
13349-82-1
The general procedure for the synthesis of 1-[2-(2-hydroxyethoxy)ethyl]piperazine from the compound (CAS:166388-52-9) was as follows: 54.2 g of compound 3 was dissolved in 300 mL of dichloromethane, followed by the addition of 26 g of trifluoroacetic acid. The reaction mixture was stirred at room temperature for 2 h. The progress of the reaction was monitored by thin layer chromatography (TLC) until the reaction was complete. After completion of the reaction, 1 N NaOH aqueous solution was added and stirring was continued for 30 minutes. The reaction mixture was left to partition and the organic phase was separated. The organic phase was dried over anhydrous sodium sulfate and subsequently concentrated under reduced pressure to give 32.6 g of a colorless liquid product, i.e., 1-[2-(2-hydroxyethoxy)ethyl]piperazine. The yield was 95%.
Yield:13349-82-1 95.1%
Reaction Conditions:
with piperazine dihydrochloride in ethanol for 10 h;Reflux;Large scale;
Steps:
5 Synthesis of N- [2- (2-hydroxyethoxy) ethyl] piperazine
Add 150 kg of 95% ethanol to the PM-RC-15 reaction tank, stir and open the feed port. Add 200 kg of piperazine bis-salt, 100 kg of piperazine to the reaction tank, dissolve it by heating, add 110 kg of chlorinated diethylene glycol, TheReaction is completed, reduced to 15-20 , centrifugal recovery of piperazine bischloride, the filtrate adjusted to pH 11, filter out sodium chloride, the filtrate vacuum distillation to collect liquid temperature of 154-160 , the top temperature of 145-148 (Yield: 95.1%) of 90 kg of N- [2- (2-hydroxyethoxy) ethyl] piperazine as a fraction (vacuum: 2 mmHg).
References:
Weinan Chang Tong Medicine Chem Technology Co.,Ltd;Chang, Shuiping CN104016945, 2016, B Location in patent:Paragraph 0039; 0040
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