(4-OXO-PIPERIDIN-1-YL)-ACETIC ACID HYDROCHLORIDE synthesis
- Product Name:(4-OXO-PIPERIDIN-1-YL)-ACETIC ACID HYDROCHLORIDE
- CAS Number:218772-96-4
- Molecular formula:C7H11NO3
- Molecular Weight:157.17
5292-43-3
40064-34-4
218772-96-4
Step 1. 4-Piperidone monohydrate hydrochloride (5 g, 0.033 mol) was mixed with tert-butyl bromoacetate (6.98 g, 0.037 mol) and potassium carbonate (13.65 g, 0.099 mol) in dimethylformamide (100 ml) and reacted for 24 hours at 100 °C. After completion of the reaction, the mixture was cooled and concentrated in vacuum. The residue was partitioned between saturated potassium carbonate solution and ether (2 x 50 ml). The organic layers were combined, dried over anhydrous sodium sulfate, filtered and evaporated to dryness to give 7.36 g of tert-butyl 2-(4-oxopiperidin-1-yl)acetate in 94% yield. The product was characterized by 1H NMR (CDCl3): δ 1.45 (9H, s), 2.45 (4H, t, J=7Hz), 2.3-2.4 (4H, m), 3.29 (2H, s).
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218772-96-4
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$76.00/100mg
Yield:218772-96-4 92.2%
Reaction Conditions:
with potassium carbonate in water at 60 - 75; for 6 h;Reagent/catalyst;Temperature;
Steps:
1 Example 1: Preparation of 4-piperidone-1-acetic acid (III)
In a 500 ml four-necked flask equipped with a stirring, thermometer, reflux condenser, and constant pressure dropping funnel,Add 60 grams of water, 34.5 grams (0.25 moles) of potassium carbonate,21.8 g (0.23 mol) of chloroacetic acid,Heat, keep between 60-65 ,A solution of 27.1 g (0.2 mole) of piperidin-4-one hydrochloride and 60 g of water was added dropwise,The addition was completed in about 2 hours, and then the reaction was stirred at 70-75 ° C for 4 hours.Cool to 20-25 ° C, 30wt% hydrochloric acid acidification system pH 2.5-3.0, filter, dry,There was obtained 28.95 g of 4-piperidone-1-acetic acid as a white solid,The yield was 92.2%, and the purity of the liquid phase was 99.3%.
References:
CN110483384,2019,A Location in patent:Paragraph 0050-0051; 0066-0067
5292-43-3
444 suppliers
$10.00/5g
40064-34-4
0 suppliers
$10.00/5g
218772-96-4
37 suppliers
$76.00/100mg