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
331443-52-8
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129306-04-3
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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
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