Formic Acid → HCID 19738500, compound
Reaction equation
[Cl:1][C:2](=[CH2:16])[CH2:3][N:4]([CH2:10][CH:11](OC)[O:12]C)[C:5](=[O:9])[O:6][CH2:7][CH3:8].C(O)=O.[Cl-].[Na+]>O>[Cl:1][C:2](=[CH2:16])[CH2:3][N:4]([CH2:10][CH:11]=[O:12])[C:5](=[O:9])[O:6][CH2:7][CH3:8]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
151 g (0.6 mol) of ethyl N-(2-chloroallyl)-N -(2,2-dimethoxyethyl)-carbamate are heated under reflux for 3 hours with 60 ml of formic acid in 1.2 1 of water. The mixture is saturated with sodium chloride, and the aqueous phase is separated off and extracted twice with 300 ml of methylene chloride each time. The organic phases are washed with saturated sodium hydrogen carbonate solution until neutral, dried over magnesium sulphate and concentrated, and the residue is distilled.
Workup
- customthe aqueous phase is separated off
- extractionextracted twice with 300 ml of methylene chloride each time
- washThe organic phases are washed with saturated sodium hydrogen carbonate solution until neutral,
- dry with materialdried over magnesium sulphate
- concentrationconcentrated
- distillationthe residue is distilled
Sources & evidence
- ORD record
- ord-48cd5603b4eb4bc1bb61f700f4785181
- Source dataset
- uspto-grants-1991_12
- Patent number
- US05071999
Reaction notes
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