Monoethyl Adipate synthesis
- Product Name:Monoethyl Adipate
- CAS Number:626-86-8
- Molecular formula:C8H14O4
- Molecular Weight:174.19
Yield:626-86-8 98.4%
Reaction Conditions:
with acetic acid in chloroform;water at 60; for 8 h;Reagent/catalyst;Temperature;Solvent;
Steps:
7 Example 7:
A)The organic layer was prepared by first heating adipic acid, 6% acetic acid by mass concentration, 95% mass concentration ethanol and water in chloroform to 60 ° C. and holding at 60 ° C. for 8 h,Adipic acid, 95% by mass of ethanol, 5% by mass of acetic acid, chloroform and water in a concentration of 6% by weight is 1: 0.45: 0.2: 4:After the insulation layering,Remove the acid layer,The acid layer is recycled to step A) of the next round of reaction, ie, to step A) for the next round of preparation of monoethyl adipate,Get organic layer;B)concentrate,The organic layer obtained in step A) was concentrated under reduced pressure,The decompression pressure was -0.085 MPa and the temperature, that is, the internal temperature was 60 ° C.,Get adipic acid monoethyl ester initial product concentrate;C)Extraction and purification,Will be obtained in step B) adipic acid monoethyl ester initial product concentrate by n-heptane extractant continuous extraction and purification extraction,The extractant continuous flow extraction and purification extraction comprises the following four steps:a)The extractant, n-heptane, is first pumped from the lower part of the extractor as a light phase,From the extractor outflow,And into the jacket of the extractor temperature of 35 ° C recycled water;b)Then the monoethyl adipate initial product concentrate and extractant are simultaneously pumped into the extractor;c)Afterwards, the light phase was obtained from the top of countercurrent extraction successively,The light phase is an impurity organic layer,And from the countercurrent extraction of the bottom to get heavy phase,The heavy phase is the liquid organic layer.d)Finally, the obtained heavy phase material organic layer was concentrated to give a mol yield of 98.4% and a purity of 99.26%Of monoethyl adipate,Light phase recovery extractant,Recycled extractant recycled.
References:
Suzhou Fushilai Pharmaceutical Co., Ltd.;Tan Xueliang;Qian Qing;Shi Xiaoqing;Shao Min;Zhang Jiayu;Ren Jian CN107043327, 2017, A Location in patent:Paragraph 0027; 0028; 0029; 0030; 0031; 0031; 0032-0082
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