These common heterocyclic compound, 2675-89-0, name is 2-Chloro-N,N-dimethylacetamide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Application In Synthesis of 2-Chloro-N,N-dimethylacetamide
Example 5.3Preparation of nC10H21-O-CH2-CONMe2 (Product 3-R1=nC10H21)In a 250 mL reactor, under a nitrogen atmosphere, is introduced sodium hydride, (60% suspended in mineral oil) (5 g, 125 mmol). This product is washed with pentane (3¡Á15 mL) and is then suspended in THF (100 g). The suspension is cooled to 0 C., n-decanol (17.4 g, 110 mmol) is introduced with a syringe. The chlorodimethylacetamide (12.1 g, 100 mmol) is then slowly added onto the mixture. The temperature of the reaction mixture is brought back to room temperature and the reaction mixture is maintained with stirring for 20 hours. The reaction mixture is neutralized with cold water (20 mL) and then this aqueous phase is extracted with dichloromethane (200 mL), the organic phase is washed with a saturated solution of NH4Cl (50 mL), a saturated solution of NaHCO3 (50 mL) and then with water (50 mL). The organic phase is dried on sodium sulfate and concentrated under reduced pressure in order to obtain 20.6 g of the expected product with a purity>98% i.e. a yield of 82%.
The synthetic route of 2-Chloro-N,N-dimethylacetamide has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Vidal, Thierry; Guglieri, Massimo; Jentzer, Olivier; US2012/302791; (2012); A1;,
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