Phosgene → Cyclohexylsulfamyl chloride

HRID 866772

反応式

HRID 866772 の反応式
[Cl-].[Cl:2]C(=[N+](C)C)Cl.C(Cl)(Cl)=O.[CH:12]1([NH:18][S:19](=[O:22])(=O)[OH:20])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1>ClCCCl>[CH:12]1([NH:18][S:19]([Cl:2])(=[O:22])=[O:20])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1

参加物

5

反応物 3

HCID 6371Phosgene2 回HCID 7533CyclamateHCID 2723945Phosgeniminium chloride

生成物 1

HCID 12914615Cyclohexylsulfamyl chloride収率 68%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

15 parts of dichloromethylenedimethylammonium chloride, suspended in 540 parts of 1,2-dichloroethane, are saturated with 40 parts of phosgene at 35° C, whilst stirring. 89.6 parts of cyclohexylsulfamic acid are now added and a further 550 parts of phosgene are then introduced in the course of 15 hours at 83° C, whilst stirring. After removing excess phosgene, and the solvent, under reduced pressure, 67.2 parts (68% of theory) of cyclohexylsulfamic acid chloride of boiling point 100°-114° C/0.01 mm Hg and melting point 43°-47° C are obtained by distillation of the residue.

後処理

  1. stirringwhilst stirring
  2. customAfter removing excess phosgene

出典と根拠

ORDレコード
ord-446bc1bbaa5e4c3fb941c130704c3038
出典データセット
uspto-grants-1978_07
特許番号
US04101571

関連ノート

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