1,2-Dichloroethane → HCID 12375834, compound
Reaction equation
N1C=CC=CC=1.[C:7]([Cl:10])(Cl)=[O:8].ClCCCl.[CH:15]([NH:18][S:19]([Cl:22])(=[O:21])=[O:20])([CH3:17])[CH3:16]>O>[Cl:10][C:7]([N:18]([CH:15]([CH3:17])[CH3:16])[S:19]([Cl:22])(=[O:21])=[O:20])=[O:8]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 22 °C
Procedure
316.4 parts of pyridine are introduced at -10° C., whilst stirring, into a solution of 400 parts of phosgene in 2,500 parts of 1,2-dichloroethane. 630.4 parts of isopropylsulfamic acid chloride are then added at the same temperature and the reaction mixture is stirred for one hour at 22° C. Thereafter, the mixture is stirred for 8 minutes with 700 parts of water at 6° C. and pH 1. The organic phase is then separated off from the 2-phase mixture formed, and is filtered and subjected to fractional distillation. 763 parts (87% of theory) of N-chlorocarbonyl-N-isopropylsulfamic acid chloride, of boiling point 57°-62° C./0.11 mbar and nD25 =1.4749, are obtained.
Workup
- customThe organic phase is then separated off from the 2-phase mixture
- customformed
- filtrationis filtered
- distillationsubjected to fractional distillation
Sources & evidence
- ORD record
- ord-fc27b1e8e0b04a9297c1506670e1951a
- Source dataset
- uspto-grants-1982_04
- Patent number
- US04327034
Reaction notes
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