![](/CAS/GIF/129306-04-3.gif)
5-Azaspiro[2.4]heptane-4,7-dione, 5-(phenylMethyl)- synthesis
- Product Name:5-Azaspiro[2.4]heptane-4,7-dione, 5-(phenylMethyl)-
- CAS Number:129306-04-3
- Molecular formula:C13H13NO2
- Molecular Weight:215.25
![Cyclopropanecarboxamide, 1-(2-bromoacetyl)-N-(phenylmethyl)-](/CAS/20210305/GIF/331443-52-8.gif)
331443-52-8
0 suppliers
inquiry
![5-Azaspiro[2.4]heptane-4,7-dione, 5-(phenylMethyl)-](/CAS/GIF/129306-04-3.gif)
129306-04-3
43 suppliers
inquiry
Yield:129306-04-3 73%
Reaction Conditions:
with tetrabutylammomium bromide;sodium hydroxide in 1,2-dichloro-ethane at 50 - 70; for 5 h;Large scale;
Steps:
1 5-Benzyl-5-azaspiro [2,4] heptane-4, 7-dione V
A solution of 1-bromo-3-cyclopropylacetoacetamide benzylamide IV (2 · 93 kg, 9.9 mol) was taken at 50 ° COf the reactor,Adding 10L of 1,2-dichloroethane, 10L of 25% NaOH and 0.45kg of tetra-n-butyl ammonium bromide. After stirring for 5 hours at 70 ° C, add 10L of water and the appropriate amount of dichloromethane, and extract the organic layer , Washed with water to near neutral, anhydrous sodium sulfate drying, steaming the solvent brown oil 2. 3kg. To the reaction mixture, 25 L of acetone and 2.5 L of 1N hydrochloric acid were added thereto. The reaction mixture was refluxed for 15 hours. The acetone was distilled off and the pH of the reaction solution was adjusted to 6-7 with NaOH solution. The dichloromethane extraction solution was washed with saturated brine and the solvent was distilled off to give a colorless oil 5-azaspiro [2,4] heptane-4, 7-dione V as a yellow crystalline solid (1.44 g, 86.4%) as a yellow crystal 1.55 kg, 73%
References:
CN103420896,2016,B Location in patent:Paragraph 0045-0046
![ethyl 1-acetylcyclopropanecarboxylate](/CAS2/GIF/32933-03-2.gif)
32933-03-2
109 suppliers
$41.00/250mg
![Benzylamine](/CAS/20180906/GIF/100-46-9.gif)
100-46-9
463 suppliers
$5.00/5G
![5-Azaspiro[2.4]heptane-4,7-dione, 5-(phenylMethyl)-](/CAS/GIF/129306-04-3.gif)
129306-04-3
43 suppliers
inquiry
![N-BENZYL-N-(TERT-BUTOXYCARBONYL)GLYCINE](/CAS/GIF/76315-01-0.gif)
76315-01-0
52 suppliers
$82.50/1g
![5-Azaspiro[2.4]heptane-4,7-dione, 5-(phenylMethyl)-](/CAS/GIF/129306-04-3.gif)
129306-04-3
43 suppliers
inquiry
![207554-16-3](/CAS/20210111/GIF/207554-16-3.gif)
207554-16-3
1 suppliers
inquiry
![5-Azaspiro[2.4]heptane-4,7-dione, 5-(phenylMethyl)-](/CAS/GIF/129306-04-3.gif)
129306-04-3
43 suppliers
inquiry