Methanol → N-methoxymethyl-N-propylsulfamic acid chloride
Reaction equation
[CH3:1][O-:2].[Na+].CO.Cl[CH2:7][N:8]([CH2:13][CH2:14][CH3:15])[S:9]([Cl:12])(=[O:11])=[O:10]>C1CCCCC1>[CH3:1][O:2][CH2:7][N:8]([CH2:13][CH2:14][CH3:15])[S:9]([Cl:12])(=[O:11])=[O:10]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 42.5 °C
Procedure
26 parts of sodium methylate in 160 parts of methanol are added in the course of 20 minutes, at from 0 to 5° C., to a mixture of 106 parts of N-chloromethyl-N-propysulfamic acid chloride in 200 parts of cyclohexane. The reaction mixture is then stirred for 1 hour at from 40 to 45° C., after which the sodium chloride which has precipitated is separated off. On subsequent distillation, the solvent is removed first and 70.5 parts (68% of theory) of N-methoxymethyl-N-propylsulfamic acid chloride of boiling point 59-65° C./0.1 mbar and nD25 = 1.4543 are then obtained.
Workup
- customafter which the sodium chloride which has precipitated
- customis separated off
- distillationOn subsequent distillation
- customthe solvent is removed first
Sources & evidence
- ORD record
- ord-dfd91dd5c07b401983b3a4b8be7f5e50
- Source dataset
- uspto-grants-1978_12
- Patent number
- US04131620
Reaction notes
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