5-(N-PHTHALIMIDO)-2-PENTANONE synthesis
- Product Name:5-(N-PHTHALIMIDO)-2-PENTANONE
- CAS Number:3197-25-9
- Molecular formula:C13H13NO3
- Molecular Weight:231.25
Yield:3197-25-9 88%
Reaction Conditions:
Stage #1: 5-chloro-2-pentanone;phthalimidewith potassium carbonate in DMF (N,N-dimethyl-formamide) at 20 - 80; for 18 - 24 h;
Stage #2: with lithium hydroxide monohydrate in DMF (N,N-dimethyl-formamide) at 0 - 5; for 1 h;
Steps:
1.1
A mixture of phthalimide (73. 5g, 0.5 mol), 5-chloro-2-pentanone (120.6g, 1 mol), potassium carbonate (105g, 0.75 mol) and N, N-dimethylformamide (500 mL) was stirred and heated to 80°C for 18-24h. After cooling to ambient temperature, the mixture was added to ice-cold water (2.5 L). The resulting suspension was stirred at 0-5°C for 1 hour, then the precipitated product was filtered off, washed thoroughly with water (1.5 L) and dried under high vacuum at 50°C for 18 hours. Yield 102g (88%) 1H NMR (400MHz) : Consistent with structure HPLC: 98.9% PAR
References:
WO2003/93239,2003,A2 Location in patent:Page/Page column 7
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