N,N-Dimethylethylenediamine → 6-Amino-2-butoxy-9-(3-{[2-(dimethylamino)ethyl]amino}propyl)-7,9-dihydro-8H-purin-8-one, hydrochloride
Reaction equation
[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:20])[N:6]2[CH2:16][CH2:17][CH2:18][Cl:19].[CH3:21][N:22]([CH3:26])[CH2:23][CH2:24][NH2:25]>CS(C)=O>[ClH:19].[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:20])[N:6]2[CH2:16][CH2:17][CH2:18][NH:25][CH2:24][CH2:23][N:22]([CH3:26])[CH3:21]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
The product of step (ii) (16 g), DMSO (16 ml) and N,N-dimethylethylenediamine (120 ml) was heated at 80° C. for 4 h then evaporated under reduced pressure. The residue was azeotroped with acetonitrile then heated under reflux in acetonitrile (250 ml) for 30 min then cooled to 0° C. for 1 h. The solid was filtered off and dried. Yield 15.32 g.
Workup
- customthen evaporated under reduced pressure
- customThe residue was azeotroped with acetonitrile
- temperaturethen heated
- temperatureunder reflux in acetonitrile (250 ml) for 30 min
- filtrationThe solid was filtered off
- customdried
Sources & evidence
- ORD record
- ord-c9ea2d24ee1745039cf96c85d5619aa6
- Source dataset
- uspto-grants-2011_11
- Patent number
- US08067411B2
Reaction notes
Loading…