ETHYL 2-(3-N-PHTHALIMIDOPROPYL)ACETOACETATE synthesis
- Product Name:ETHYL 2-(3-N-PHTHALIMIDOPROPYL)ACETOACETATE
- CAS Number:55747-45-0
- Molecular formula:C17H19NO5
- Molecular Weight:317.34
85-41-6
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141-97-9
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142-28-9
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55747-45-0
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Yield:55747-45-0 96.2%
Reaction Conditions:
Stage #1: phthalimidewith potassium carbonate in acetonitrile at 20; for 0.5 h;
Stage #2: 1,3-Dichloropropanewith sodium iodide in acetonitrile at 58 - 60; for 5.5 h;
Stage #3: ethyl acetoacetate in acetonitrile at 20; for 7 h;Reagent/catalyst;
Steps:
1.1; 2; 3; 4; 5
Add 500mL of acetonitrile, 100g of phthalimide and 281.8g of potassium carbonate to the reaction vessel, stir at room temperature for 30min, and then add 115.19g of 1,3-dichloropropane and 152.82g of sodium iodide to it; feed After completion, gradually raise the temperature to 58-60 ° C and stir the reaction for 5.5h in this temperature range, and sample to monitor the reaction of the raw material phthalimide.Then 132.68 g of ethyl acetoacetate was weighed and slowly added dropwise to the above reaction solution. After the addition was completed, the reaction was continued for 7 hours;Reduce the reaction solution to room temperature.It was filtered and the mother liquor was concentrated to dryness to obtain 207.5 g of pure compound I, with a yield of 96.2%.
References:
CN110818610,2020,A Location in patent:Page/Page column 8-9
42251-84-3
63 suppliers
$85.00/250mg
141-97-9
788 suppliers
$5.00/25g
55747-45-0
31 suppliers
$43.00/5g
85-41-6
476 suppliers
$9.00/1g
55747-45-0
31 suppliers
$43.00/5g