Ethyl 3-amino-3-methylbutanoate → Ethyl 3-[(4-bromobutyl)aminocarbonylamino]-3-methylbutanoate
Reaction equation
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]=[C:7]=[O:8].[NH2:9][C:10]([CH3:18])([CH3:17])[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13]>C(Cl)Cl>[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][NH:6][C:7]([NH:9][C:10]([CH3:18])([CH3:17])[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:8]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- -20 °C
Procedure
A solution of 4-bromobutylisocyanate (15.1 g) in methylene chloride (50 ml) is added to a stirred solution of ethyl 3-amino-3-methylbutanoate (12.3 g), dissolved in methylene chloride (50 ml) at -20° C. The mixture is stirred for 30 minutes at -20° C. and then for an additional 2 hours at room temperature. Evaporation of the solvent yields a residue of ethyl 3-[(4-bromobutyl)aminocarbonylamino]-3-methylbutanoate (26 g).
Workup
- waitfor an additional 2 hours at room temperature
- customEvaporation of the solvent
Sources & evidence
- ORD record
- ord-d021e12515424ff3a33414c07576d365
- Source dataset
- uspto-grants-1987_09
- Patent number
- US04696927
Reaction notes
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