PENTOBARBITAL-D5 synthesis
- Product Name:PENTOBARBITAL-D5
- CAS Number:73738-05-3
- Molecular formula:C12H7D5N2O3
- Molecular Weight:237.27
73738-03-1
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73738-05-3
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Yield:73738-05-3 19 g
Reaction Conditions:
Stage #1: Ethyl-d(5)-phenylmalonsaeurediethylester;ureawith sodium ethanolate in ethanol; for 1 h;Reflux;
Stage #2: with hydrogenchloride in water; pH=2;
Steps:
2.2
(2) EtONa (250.0 mmol, 17.0 g) and urea (140 mmol, 8.4 g) were further added to the reaction system, and the reaction mixture was rapidly heated to reflux. After stirring for 1 h, ethanol was distilled off under reduced pressure, and 300 mL was added to the residue. The water was stirred well, and hydrochloric acid (concentration: 6 mol / L) was added to adjust the pH to 2.It was then extracted three times with ethyl acetate. Each extraction was extracted with 300 mL of ethyl acetate. The combined organic phases were dried over anhydrous sodium sulfate (400 g), filtered, concentrated under reduced pressure, and recrystallized from ethyl acetate and petroleum ether. D5-deuterated phenobarbital 19.0g product, yield 80%.
References:
CN110467575,2019,A Location in patent:Paragraph 0029; 0034-0036
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73738-05-3
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