1-Boc-3-piperidone synthesis
- Product Name:1-Boc-3-piperidone
- CAS Number:98977-36-7
- Molecular formula:C10H17NO3
- Molecular Weight:199.25
Refining: with 1-BOC-3-piperidone crude product is that 60pa, temperature are to distill under 104 ~ 105 ℃ the condition at pressure, gets 1-BOC-3-piperidone elaboration 163g, 92.9%.
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Yield:98977-36-7 99.4%
Reaction Conditions:
with sodium hypochlorite solution;sodium hydrogencarbonate;potassium bromide in dichloromethane at 5 - 10; pH=8.5;Reagent/catalyst;
Steps:
2.2 Preparation of N-BOC-3-piperidone
In the step 2, the compound N-BOC-3-piperidone is prepared according to the following scheme:To the reaction flask was added 20.1 g of N-BOC-3-hydroxypiperidine,703.5 mg of PS-ABNO,100 ml of dichloromethane,1g of potassium bromide dissolved in water was added to the reaction system,Cooled to 5 ° C with an ice bath,8.4 g of NaHCO3 was dissolved in 100 ml of sodium hypochlorite solution,Adjust its pH = 8.5 or so,Slowly added to control the drip rate so that the reaction temperature is not higher than 10 , after the addition was completed,TLC detection, the reaction was completed, the recovery of PS-ABNO filtration, the reaction liquid was separated and the aqueous phase was extracted with 100ml of dichloromethane, the organic phase was combined, washed once with 100ml of water, the organic phase was dried over anhydrous Na2SO4, filtered, Concentration of 19.8g of light yellow oily product, to obtain the target product N-BOC-3-piperidone, yield 99.4%
References:
CN107573278,2018,A Location in patent:Paragraph 0055; 0059-0061; 0076-0077
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98977-36-7
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