Butanoic acid, 3-oxo-, 1-(phenylmethyl)-3-piperidinyl ester synthesis
- Product Name:Butanoic acid, 3-oxo-, 1-(phenylmethyl)-3-piperidinyl ester
- CAS Number:85387-34-4
- Molecular formula:C16H21NO3
- Molecular Weight:275.34
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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