Thionyl Chloride → 1-(3-chloropropyl)-1,3-dihydro-5-(trifluoromethyl)-2H-benzimidazol-2-one

HRID 46844노트

반응식

HRID 46844 반응식
O[CH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]([F:17])([F:16])[F:15])=[CH:13][C:8]=2[NH:7][C:6]1=[O:18].S(Cl)([Cl:21])=O>ClC(Cl)Cl>[Cl:21][CH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]([F:17])([F:16])[F:15])=[CH:13][C:8]=2[NH:7][C:6]1=[O:18]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 203856341,3-dihydro-1-(3-hydroxypropyl)-5-(trifluoromethyl)-2H-benzimidazol-2-one

생성물 1

HCID 203855741-(3-chloropropyl)-1,3-dihydro-5-(trifluoromethyl)-2H-benzimidazol-2-one수율 56%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a stirred mixture of 23 parts of 1,3-dihydro-1-(3-hydroxypropyl)-5-(trifluoromethyl)-2H-benzimidazol-2-one in 150 parts of trichloromethane are added dropwise 32 parts of sulfinyl chloride. Upon completion, the whole is heated to reflux and stirring is continued for 1 hour at reflux temperature. After cooling, the reaction mixture is evaporated and the residue is crystallized from 2,2'-oxybispropane, yielding 14 parts (56%) of 1-(3-chloropropyl)-1,3-dihydro-5-(trifluoromethyl)-2H-benzimidazol-2-one.

후처리

  1. temperatureUpon completion, the whole is heated
  2. temperatureto reflux
  3. temperatureat reflux temperature
  4. temperatureAfter cooling
  5. customthe reaction mixture is evaporated
  6. customthe residue is crystallized from 2,2'-oxybispropane

출처 및 근거

ORD 기록
ord-9b77ae0b880f4839ae228a99d08f44fb
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04175129

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