2,4-Dichloro-5-nitropyrimidine synthesis
- Product Name:2,4-Dichloro-5-nitropyrimidine
- CAS Number:49845-33-2
- Molecular formula:C4HCl2N3O2
- Molecular Weight:193.98
611-08-5
381 suppliers
$5.00/5g
49845-33-2
374 suppliers
$5.00/1g
Yield:49845-33-2 80%
Reaction Conditions:
with trichlorophosphate in N,N-dimethyl-formamide at 50 - 100; for 0.0833333 h;Green chemistry;
Steps:
1-3 Example 1
In a four-necked flask equipped with a thermometer, a condenser and a stirred 2000 ML,260 g of 5-nitrouracil was added, 1000 g of phosphorus oxychloride was added, and the temperature was raised to 50 ° C.Control 50 ° C ~ 100 ° C,Add 25 grams of DMF, and return to reflux after 5 minutes.The reaction was stopped when the product content in the gas phase tracking reaction solution was 95% or more.At the end of the reaction, phosphorus oxychloride was recovered under reduced pressure until a solid precipitated. Under cooling, 600 g of dichloroethane was added, stirred for 10 minutes, poured into 500 g of ice water, and the layers were stirred.The dichloroethane layer is added with 10 g of activated carbon and heated at 50 ° C to 70 ° C, stirred for 10 to 30 minutes, filtered, and added with 20 g of anhydrous sodium sulfate to dry, and the dichloroethane is recovered and distilled under reduced pressure.The finished product of 2,4-dichloro-5-nitropyrimidine was 255 g, the content was 98.5%, and the yield was 80%.
References:
Huai'an Wan Bang Flavors Co., Ltd.;Jiang Kun;Xu Shaoqiang;Yang Li CN109293578, 2019, A Location in patent:Paragraph 0012-0020
611-08-5
381 suppliers
$5.00/5g
49845-33-2
374 suppliers
$5.00/1g
611-08-5
381 suppliers
$5.00/5g
49845-33-2
374 suppliers
$5.00/1g
611-08-5
381 suppliers
$5.00/5g
49845-33-2
374 suppliers
$5.00/1g