Reaction equation
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([CH3:9])[N:3]=1.[OH-].[NH4+:11]>>[Cl:1][C:2]1[N:3]=[C:4]([CH3:9])[N:5]=[C:6]([NH2:11])[CH:7]=1Participants
3
Procedure
Charge a 5 L steel pressure vessel (autoclave) with 4,6-dichloro-2-methylpyrimidine (400 g, 2.45 mol) and ammonium hydroxide (2.8 L) at RT. Heat the reaction to 90° C. for 5 h. Cool the reaction mixture to RT and then filter the solid through a Buchner funnel. Wash the filtercake with water (200 mL) and hexane (200 mL) and then dry under vacuum to afford the title compound as a white solid (290 g, 82%). LC-ES/MS m/z 144.0 (M+1).
Workup
- temperatureHeat
- customthe reaction to 90° C. for 5 h
- filtrationfilter the solid through a Buchner funnel
- washWash the filtercake with water (200 mL) and hexane (200 mL)
- customdry under vacuum
Sources & evidence
- ORD record
- ord-889e43dc4de442488dae8be6d25a24e1
- Source dataset
- uspto-grants-2015_05
- Patent number
- US09035051B1
Linked notes
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