Ethyl chloroformate → N-(1,1-dimethoxyprop-2-yl)urethane
Reaction equation
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[CH3:7][O:8][CH:9]([O:13][CH3:14])[CH:10]([NH2:12])[CH3:11].[OH-].[Na+]>C1(C)C=CC=CC=1.O>[CH3:7][O:8][CH:9]([O:13][CH3:14])[CH:10]([NH:12][C:2]([O:4][CH2:5][CH3:6])=[O:3])[CH3:11]Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Procedure
80 g (0.73 mol) of ethyl chloroformate are added dropwise to 86.2 g (0.72 mol) of 2-aminopropionaldehyde dimethyl acetal in 350 ml of toluene and 32 g (0.8 mol) of NaOH in 300 ml of water. The mixture is stirred at room temperature for a further 2 hours, the organic phase is separated off, the aqueous phase is extracted with toluene and the toluene solutions are dried over K2CO3. The solution is concentrated and the residue is distilled.
Workup
- customthe organic phase is separated off
- extractionthe aqueous phase is extracted with toluene
- dry with materialthe toluene solutions are dried over K2CO3
- concentrationThe solution is concentrated
- distillationthe residue is distilled
Sources & evidence
- ORD record
- ord-acd54b968634414ab260eeadb9f96832
- Source dataset
- uspto-grants-1995_05
- Patent number
- US05416096
Reaction notes
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