Phosphorus pentachloride → Butylsulfamyl chloride

HRID 1823134ノート

反応式

HRID 1823134 の反応式
[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

反応物 2

HCID 24819Phosphorus pentachlorideHCID 3628384butylsulfamic acid

生成物 1

HCID 13544378Butylsulfamyl chloride

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

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

  1. temperaturewas warmed gently
  2. customresulted
  3. temperatureThe cloudy solution was heated
  4. temperatureto reflux for 0.5 h.
  5. concentrationwas concentrated

出典と根拠

ORDレコード
ord-c0a4fef436f341128bb3387803199d23
出典データセット
uspto-grants-2006_05
特許番号
US07037941B2

反応ノート

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