tert-butyl 7-azabicyclo[4.1.0]heptane-7-carboxylate synthesis
- Product Name:tert-butyl 7-azabicyclo[4.1.0]heptane-7-carboxylate
- CAS Number:153789-13-0
- Molecular formula:C11H19NO2
- Molecular Weight:197.27
![7-Aza-bicyclo[4.1.0]heptane](/CAS/GIF/CB22369411.gif)
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Yield:153789-13-0 92.2%
Reaction Conditions:
with N,N-dimethyl-4-aminopyridine;triethylamine in dichloromethane at 0 - 20; for 8 h;
Steps:
1 Example 1:
Put 7-azabicyclo[4.1.0]heptane (97.2g, 1.0mol) into the reaction flask, DMAP2.2g, di-tert-butyl dicarbonate (261.9g, 1.2mol) were dissolved in dichloromethane 600mL. The temperature was controlled at 0-5°C, triethylamine (126.5g, 1.25mol) was added dropwise, the temperature was naturally raised to room temperature for 8 hours after dropping, and the reaction was completed by TLC detection, and 1M hydrochloric acid was adjusted to pH=7-8 for layering,Extracted with 400 mL of dichloromethane, combined the organic phases, washed with 200 mL of 20% aqueous potassium hydrogen sulfate solution, washed with saturated aqueous sodium carbonate solution, dried over anhydrous sodium sulfate, concentrated under reduced pressure,Under reduced pressure distillation at 55-60° C. to obtain 182.1 g of tert-butyl 7-azabicyclo[4.1.0]heptane-7-carboxylate with a yield of 92.2% and a chemical purity of 99.4%.
References:
CN113999142,2022,A Location in patent:Paragraph 0021-0023
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153789-13-0
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153789-13-0
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