Phosphorus pentachloride → n-Butylsulfamoyl chloride
Reaction equation
[CH2:1]([NH:5][S:6](=[O:9])(=O)[OH:7])[CH2:2][CH2:3][CH3:4].P(Cl)(Cl)(Cl)(Cl)[Cl:11]>C1C=CC=CC=1>[CH2:1]([NH:5][S:6]([Cl:11])(=[O:9])=[O:7])[CH2:2][CH2:3][CH3:4]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A suspension of n-butyl sulfamic acid (1.92 gm, 12.53 mmoles) and phosphorus pentachloride 2.61 gm, 12.53 mmoles) in benzene (20.mL) was warmed gently to initiate gas evolution. The reaction mixture was stirred at room temperature for 0.5 h., during which time a cloudy solution resulted. The cloudy solution was heated to reflux for 0.5 h., then was concentrated. The product n-butyl sulfamoyl chloride was isolated by vacuum distillation (120° C., 300 millitorr), 730 mg (liq.) (34%).
Workup
- temperaturewas warmed gently
- customresulted
- temperatureThe cloudy solution was heated
- temperatureto reflux for 0.5 h.
- concentrationwas concentrated
Sources & evidence
- ORD record
- ord-8904ec8ca4d74c2d944233eb9e4edb95
- Source dataset
- uspto-grants-2000_12
- Patent number
- US06156768
Reaction notes
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