Hydrazine hydrate (1:1) → 4-Chloro-6-hydrazinylpyrimidine

With stirring and at RT, 11.8 ml (12.1 g, 241.6 mmol) of hydrazine hydrate are added dropwise to a solution of 20.0 g (134.3 mmol) of 4,6-dichloropyrimidine in 300 ml of ethanol. If the solution becomes turbid during the addition of the hydrazine hydrate, more solvent (about 400 ml of ethanol) is added. The reaction solution is stirred at RT for a further 12 h. For work-up, the precipitated solid is filtered off, the filter residue is washed twice with in each case 150 ml of water and twice with in each case 100 ml of diethyl ether and the product is dried under reduced pressure. A further crystalline fraction is obtained from the concentrated mother liquor.

1. additionis added
2. stirringThe reaction solution is stirred at RT for a further 12 h
3. filtrationFor work-up, the precipitated solid is filtered off
4. washthe filter residue is washed twice with in each case 150 ml of water and twice with in each case 100 ml of diethyl ether
5. customthe product is dried under reduced pressure
6. customA further crystalline fraction is obtained from the concentrated mother liquor

ORDレコード

ord-037a18a4ceb64266ba6db29d22c9f1eb

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08524699B2