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ChemicalBook CAS DataBase List 4-Bromomethyl-1,2-dihydroquinoline-2-one
4876-10-2

4-Bromomethyl-1,2-dihydroquinoline-2-one synthesis

3synthesis methods
The improvement compound synthesis method of a 4-bromomethyl quinoline-2 (H) ketone gets the acetyl bromide phenyl methyl ketone by alpha-acetylacetanilide bromination reaction in chloroform, and cyclization makes in the vitriol oil then; It is characterized in that: in described bromination reaction, controlled temperature is no more than 30 ℃, slowly adds the chloroformic solution of dissolving bromine; Add 20-30 ℃ and stir 2-3h; Slowly be warming up to 60-65 ℃, stir, insulation 0.5-1h.
1205-74-9 Synthesis
4-Bromo-3-oxo-N-phenylbutanamide

1205-74-9
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Yield:4876-10-2 95.08%

Reaction Conditions:

with phosphorus pentoxide at 83; for 13 h;Flow reactor;Large scale;Solvent;

Steps:

1 Example 1
In the 5000L enamel reactor,After 4000 kg of dichloroethane was charged,500 kg of acetoacetanilide bromide,Stirring evenly;At the same time in another 2000L reactor in 1000 kg of dichloroethane and 1000 kg of phosphorus pentoxide,Began at the same time will 5000L reactor and 2000L reactor temperature to dichloroethane reflux,The reaction temperature was 83 .After refluxing for one hour,5000L distillation reactor out of the dichloroethane condensate into the 2000L reactor,2000L reactor dehydration distillation of dichloroethane condensate into the 5000L reactor,Control two kettle distillation speed synchronization;After 12 hours of reaction,Cooling to room temperature;The 4-bromomethylquinolinone was separated by a filter press,The 4-bromomethylquinolinone was further washed with dichloroethane,And then through the filter press after separation,The obtained wet product containing dichloroethane solvent was vacuum dried,442 kg of white powdery solid;The yield was 95.08% and the purity was 99.67% (HPLC).

References:

Chen, Ke;Wu, Xiongfei CN105753781, 2016, A Location in patent:Paragraph 0016; 0017

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