4-Ethyl-2,3-dioxo-1-piperazine carbonyl chloride synthesis
- Product Name:4-Ethyl-2,3-dioxo-1-piperazine carbonyl chloride
- CAS Number:59703-00-3
- Molecular formula:C7H9ClN2O3
- Molecular Weight:204.61
32315-10-9
415 suppliers
$10.00/1g
59702-31-7
257 suppliers
$43.60/10g
59703-00-3
231 suppliers
$90.00/1 g
Yield:59703-00-3 94.3%
Reaction Conditions:
with pyridine;dmap;chloro-trimethyl-silane in dichloromethane at -25 - -20;
Steps:
1.1-3.1; 1.1 Example 1: (improved)
1) taking N-ethyldioxypiperazine 14.2 g (0.10 mol),Transfer to a 500 mL three-necked flask, stir, and add 200 mL of dichloromethane.Cool down to -25 to -20 ° C, add 16.3 g (0.15 mol) TMCS,Control temperature -25 ~ -20 ° C, add 11.9g (0.15mol) pyridine,Adding 0.018 g of DMAP, adding 11.9 g (0.04 mol) of triphosgene in batches at a temperature of -25 to -20 ° C, and maintaining the reaction for 30-60 minutes;After the reaction was completed, suction filtration, washing with 30 mL of dichloromethane and distillation to dryness under reduced pressure.Add 100 mL of n-hexane to crystallize and filter by suction.Drying gave 19.3 g of N-ethylbisoxypiperazine chloride in a yield of 94.3%.
References:
Qilu Tianhe Huishi (Leling) Pharmaceutical Co., Ltd.;Qilu Tianhe Huishi Pharmaceutical Co., Ltd.;Sun Zhengjun;Fan Changying;Sun Yue;Li Yong CN109734725, 2019, A Location in patent:Paragraph 0028-0029; 0031-0032; 0034-0035; 0037-0038; 0041
