Diisopropyl malonate synthesis
- Product Name:Diisopropyl malonate
- CAS Number:13195-64-7
- Molecular formula:C9H16O4
- Molecular Weight:188.22
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Yield:-
Reaction Conditions:
Stage #1:cyanoacetic acid;isopropyl alcohol at 90; for 3 h;
Stage #2:ethanol with hydrogenchloride in water at 50; for 5 h;
Steps:
3 Example 3 A method for preparing diisopropyl malonate:
1) Esterification The 70wt% concentration of cyanoacetic acid was mixed with the corresponding isopropanol to carry out the esterification reaction. The temperature was 90° C. and the temperature was maintained for 3 hours. The esterification reaction was completed; the molar ratio of cyanoacetic acid:isopropanol was 1:1.1.2) Dehydration waterAfter the reaction, the material is kept at a temperature of 60°C and subjected to normal pressure and vacuum distillation to remove excess alcohol and water in the material and control the moisture content of the alcohol end point material to be ≤ 3%;3) Alcoholysis esterificationThe dealcoholated material was maintained at a temperature of 50°C, then a hydrogen chloride-isopropanol solution was added and reacted at 50°C for 5 hours; the molar ratio of cyanoacetic acid:hydrogen chloride:isopropanol was 1:1.6:1.9. 4) Crude ester separationAfter the alcoholysis was completed, the material was cooled to 40°C, ammonia water was adjusted to pH 7.2, and the alcohol was degassed at regular pressure.Afterwards, the temperature was lowered to 34° C., water-soluble salt was added, and the ester layer and the salt water layer were separated after standing. The ester layer was distilled to obtain the malonate ester product.
References:
Weifang Binhai Petrochemical Co., Ltd.;Dou Rongtan;Lin Xiaopeng;Sun Zhenmin;Li Jianming;Song Shuai;Wang Tingwei CN107540543, 2018, A Location in patent:Paragraph 0059-0068
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