3,3-Dichloro-1-(4-nitrophenyl)piperidin-2-one synthesis
- Product Name:3,3-Dichloro-1-(4-nitrophenyl)piperidin-2-one
- CAS Number:881386-01-2
- Molecular formula:C11H10Cl2N2O3
- Molecular Weight:289.11
38560-30-4
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Yield:881386-01-2 94.9%
Reaction Conditions:
with phosphorus(V) chloride in chlorobenzene at 55; for 5 h;
Steps:
1 Synthesis of 3,3-dichloro-1-(4-nitrophenyl)piperidin-2-one
Compound II (40 g, 0.18 mol) was added to a 1000 mL eggplant-Chlorobenzene (400 ml),Phosphorus pentachloride (132.4 g, 0.64 mol) was added portionwise with stirring,After the addition warmed to 55 reaction 5h.The reaction solution was cooled to room temperature,Poured into 1000mL ice water,Separate the lower, and then extracted with dichloromethane 3 × 200mL,The combined organic phases were washed twice with 2 × 200 mL of water,400mL saturated brine was washed once,Dried over anhydrous sodium sulfate,Dichloromethane evaporated to give the product,Light yellow solid, 49.4 g, m.p.115-117°C, Yield 94.9%.
References:
CN107400131,2017,A Location in patent:Paragraph 0026; 0031; 0036-0038
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