Phosgene → Cyclohexylsulfamyl chloride

HRID 866773

反応式

HRID 866773 の反応式
CN(C)C([Cl:5])=O.C(Cl)(Cl)=O.[CH:11]1([NH:17][S:18](=[O:21])(=O)[OH:19])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1>ClCCCl>[CH:11]1([NH:17][S:18]([Cl:5])(=[O:21])=[O:19])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1

参加物

5

反応物 3

HCID 6371Phosgene3 回HCID 6598Dimethylcarbamoyl ChlorideHCID 7533Cyclamate

生成物 1

HCID 12914615Cyclohexylsulfamyl chloride収率 58%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
83 °C

実験手順

A solution of 15 parts of dimethylcarbamic acid chloride in 310 parts of 1,2-dichloroethane is saturated with 30 parts of phosgene at 25° C and 89.5 parts of cyclohexylsulfamic acid are then added. The reaction mixture is heated to 83° C whilst continuing to introduce phosgene. In total, 330 parts of phosgene are introduced in the course of 13 hours. After removing the solvent and the dimethylcarbamic acid chloride under reduced pressure, the residue is distilled, and 57 parts (58% of theory) of cyclohexylsulfamic acid chloride of boiling point 208°-127° C/0.1 mm Hg and melting point 42°-44° C are obtained.

後処理

  1. customAfter removing the solvent
  2. distillationthe dimethylcarbamic acid chloride under reduced pressure, the residue is distilled

出典と根拠

ORDレコード
ord-bd6bdfb9311641829d0d03b08693b735
出典データセット
uspto-grants-1978_07
特許番号
US04101571

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