Ethylamine → HCID 18504782, compound
Reaction equation
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4](Cl)[N:3]=1.[CH2:12]([NH2:14])[CH3:13]>C(O)CCC>[CH2:12]([NH:14][C:4]1[N:3]=[C:2]([Cl:1])[N:10]=[C:9]2[C:5]=1[NH:6][CH:7]=[N:8]2)[CH3:13]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 84 °C
Procedure
To a suspension of 2,6-dichloropurine (2 g, 10.6 mmol) in n-butanol (3 ml), is added ethylamine (2M in THF)(15 ml). The solution is stirred at 84° C. for 2.5 hours and then cooled to ambient and stirred for a further 2 hours. The resulting precipitate is isolated by filtration, washed with n-butanol, methanol and ethyl acetate. The solid is dried at 70° C., under vacuum, for 16 hours to give 6-ethylamino-2-chloropurine; ES+ (M+1)197.5,198.2; mp 237-239° C.
Workup
- temperaturecooled
- stirringstirred for a further 2 hours
- customThe resulting precipitate is isolated by filtration
- washwashed with n-butanol, methanol and ethyl acetate
- customThe solid is dried at 70° C., under vacuum, for 16 hours
Sources & evidence
- ORD record
- ord-7114661dbbb84df2b70b984e3dfa2ee1
- Source dataset
- uspto-grants-2003_07
- Patent number
- US06589950B1
Reaction notes
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