Hydrochloric Acid → 5-[4-(4-Chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine hydrochloride
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][C:15]3[C:16]([NH2:22])=[N:17][C:18]([NH2:21])=[N:19][CH:20]=3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.Cl>CO>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][C:15]3[C:16]([NH2:22])=[N:17][C:18]([NH2:21])=[N:19][CH:20]=3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1Participants
4
Procedure
0.18 g (0.00056 mol) of 5-[4-(4-chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine was dissolved in 250 ml of hot methanol. The solution was treated at room temperature with 0.32 ml (0.00112 mol) of 3.5N ethanolic hydrochloric acid. The solution was completely freed from the solvents and the residue was recrystallized from methanol/diethyl ether. 0.22 g (100%) of 5-[4-(4-chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine hydrochloride (1:1.9) was obtained as white crystals; m.p. 252°-253°.
Workup
- customthe residue was recrystallized from methanol/diethyl ether
Sources & evidence
- ORD record
- ord-9c45314138d041139465dd87c55045b8
- Source dataset
- uspto-grants-1997_11
- Patent number
- US05688798
Reaction notes
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