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

11.8 ml (12.1 g, 241.6 mmol) hydrazine hydrate are added dropwise to a solution of 20.0 g (134.3 mmol) 4,6-dichloropyrimidine in ethanol at RT, while stirring. If clouding of the solution occurs during metering in of the hydrazine hydrate, further ethanol (approx. 400 ml) is added. The reaction solution is subsequently stirred at RT for 12 h. For working up, the solid which has precipitated out is filtered off, the residue on the filter is washed twice with 150 ml water each time and twice with 100 ml diethyl ether each time and the product is dried in vacuo. A further crystalline product fraction is obtained from the concentrated mother liquor.

1. additionis added
2. stirringThe reaction solution is subsequently stirred at RT for 12 h
3. customthe solid which has precipitated out
4. filtrationis filtered off
5. washthe residue on the filter is washed twice with 150 ml water each time
6. dry with materialtwice with 100 ml diethyl ether each time and the product is dried in vacuo
7. customA further crystalline product fraction is obtained from the concentrated mother liquor

ORDレコード

ord-1facbe122c9b4e5fa1c20e9e1f5f47d3

出典データセット

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08653111B2