4,6-Dichloropyrimidine synthesis

14synthesis methods

Product Name:4,6-Dichloropyrimidine
CAS Number:1193-21-1
Molecular formula:C4H2Cl2N2
Molecular Weight:148.98

The synthesis of 4,6-Dichloropyrimidine is as follows:Dissolve 105.5g of 4,6-diaminopyrimidine in 660.0g of 31% hydrochloric acid and pour into a 2000ml bottle to cool to -5 ° C and dropwise add 500.3g of 33% sodium nitrite. After 2 hours of reaction, HPLC detects 4,6-diamino Pyrimidine is less than 0.5%. 42.8 g of cuprous chloride and 214.0 g of 31% hydrochloric acid are prepared in a 2000 ml bottle. The diazonium salt mother liquor is added dropwise to the bottle. After the dropwise reaction, the reaction is performed at 45 ° C for 2 hours. .Extract with 400g of recovered trichloroethane (200x2 times less than new ones), combine the organic layers for distillation, control the water flush pump 5KPa, temperature 40-140 , collect 404.2g of solvent in the early 40-90 , 90-140 in the later The product was collected at a temperature of 14 ° C to obtain 146.9 g of 4,6-dichloropyrimidine. The yield was 86.4% (based on formazan hydrochloride) and the purity was 99.4%.

104-90-5 Synthesis

104-90-5
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$14.00/5mL

1193-24-4
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$6.00/25g

1193-21-1
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$14.00/5g

Yield:1193-21-1 100%

Reaction Conditions:

with trichlorophosphate

Steps:

2 Example 2

Example 2 2680 g of phosphorus oxychloride were initially introduced into the reaction vessel and 980 g of 2-methyl-5-ethyl-pyridine were added, while cooling. 460 g of 4,6-dihydroxypyrimidine were then metered in over a period of 1 hour. Further reaction and working up were carried out as described in Example 1. 4,6-Dichloropyrimidine was obtained in a yield of virtually 100% and 88% by weight of the amount of amine employed was recovered.

References:

US5719285,1998,A

1193-24-4
565 suppliers
$6.00/25g

1193-21-1
570 suppliers
$14.00/5g

References

2434-56-2 Synthesis