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ChemicalBook CAS DataBase List Butanoic acid, 3-oxo-, 1-(phenylmethyl)-3-piperidinyl ester
85387-34-4

Butanoic acid, 3-oxo-, 1-(phenylmethyl)-3-piperidinyl ester synthesis

10synthesis methods
14813-01-5 Synthesis
1-Benzyl-3-piperidinol

14813-01-5
330 suppliers
$9.00/1g

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Yield:85387-34-4 786.1 g

Reaction Conditions:

with boric acid in toluene;Reflux;

Steps:

3 Preparation of (1-benzyl-3-piperidyl) acetoacetate

1-Benzyl-3-piperidinol (600 g), toluene (6 L), ethyl acetoacetate (490.2 g), boric acid (19.5 g) were added to a 10 L reaction flask. Heated to reflux overnight, HPLC detection, The remaining 2-6.2% of 3-benzyl-3-piperidinol was added to the atmospheric distillation apparatus to distill off the ethanol produced by the reaction. Complete the reaction in 2 hours, cool to 0~10 °C, adjust the pH to about 3, and extract the product with water (1 L × 2). The aqueous phase was combined, and the pH of the aqueous phase was adjusted to about 7 and extracted with ethyl acetate (1L×2). Wash with saturated brine (500 mL×2), dry over anhydrous sodium Concentrated to dryness afforded 786.1 g of a yellow oil.

References:

CN104529872,2018,B Location in patent:Paragraph 0040-0042

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