Phosphorus pentachloride → Butylsulfamyl chloride
反応式
[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]参加物
4
実験手順
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%).
後処理
- temperaturewas warmed gently
- customresulted
- temperatureThe cloudy solution was heated
- temperatureto reflux for 0.5 h.
- concentrationwas concentrated
出典と根拠
- ORDレコード
- ord-66518caf73794347ac44cfc98bb0a2db
- 出典データセット
- uspto-grants-2002_09
- 特許番号
- US06444678B1
反応ノート
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