TRIETHYL 4-PHOSPHONOCROTONATE synthesis
- Product Name:TRIETHYL 4-PHOSPHONOCROTONATE
- CAS Number:10236-14-3
- Molecular formula:C10H19O5P
- Molecular Weight:250.23
Yield: 93%
Reaction Conditions:
in toluene at 170; under 3750.38 - 15001.5 Torr; for 0.25 h;Large scale;Arbuzov Reaction;
Steps:
16 Example 16
The dry and clean 500mL coil was heated to 170 , take Compound 15 (standard atmospheric pressure boiling point of 210 ~214 ° C) 1000g (0.7eq.5.18mol) placed in a feeding bottle A, adding 4000g toluene diluted to take triethyl phosphite (the standard Atmospheric pressure boiling point 156.6 ° C) 1210g (1.0eq.7.25mol) placed in the bottle B, 3790g of toluene was added to be diluted until The coil was started and the temperature was stable. Pump A (compound 15 in toluene): 16.7 g / min, pump B (trimethyl phosphite):16.7 g / min. Residence time 15min, the reaction pressure is 0.5 ~ 2.0Mpa. The discharge port is directly connected to the thin film evaporation device, control The pressure of 4 ~ 10 × 102Pa, the temperature of 150 ~ 160 , the final product 16 (boiling point 194 ~ 198 , 800Pa) 1210g, Yield 93%.
References:
Kailaiying Life Science And Technology (Tianjin) Co., Ltd.;Hong Hao;Zhan Musi·gaiji;Lu Jiangping;Li Chao;Zhang Enxuan CN107163079, 2017, A Location in patent:Paragraph 0092; 0093; 0094; 0095
623-73-4
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$26.69/5g
682-30-4
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$34.93/1G
10236-14-3
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$50.00/2 g