Phosgene → Cyclohexylsulfamyl chloride

HRID 866773

반응식

HRID 866773 반응식
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

참가 물질

5

반응물 3

HCID 6371Phosgene3회HCID 6598Dimethylcarbamoyl ChlorideHCID 7533Cyclamate

생성물 1

HCID 12914615Cyclohexylsulfamyl chloride수율 58%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
83 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-bd6bdfb9311641829d0d03b08693b735
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04101571

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