Dimethyl Sulfoxide → Hexadecylpyridinium Sulfacetamide

HRID 2403114노트

반응식

HRID 2403114 반응식
[Cl-].[CH2:2]([N+:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[CH3:24][C:25]([N-:27][S:28]([C:31]1[CH:32]=[CH:33][C:34]([NH2:37])=[CH:35][CH:36]=1)(=[O:30])=[O:29])=[O:26].[Na+].C(Cl)(Cl)Cl.CS(C)=O>O>[CH2:2]([N+:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[CH3:24][C:25]([NH:27][S:28]([C:31]1[CH:36]=[CH:35][C:34]([NH2:37])=[CH:33][CH:32]=1)(=[O:30])=[O:29])=[O:26]

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 6212ChloroformHCID 31239Cetylpyridinium ChlorideHCID 4022878Sodium Sulfacetamide

생성물 1

HCID 69294845Hexadecylpyridinium Sulfacetamide수율 99.22%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Hexadecylpyridinium chloride (0.001 mol) was dissolved in 60 mL of distilled water by gentle heating and stirring. Sodium sulfacetamide (0.001 mol) was dissolved in 60 mL of distilled water by gentle heating and stirring. The two solutions were combined and the reaction mixture was heated and stirred for 30 minutes. The reaction mixture cooled to room temperature and then 60 mL of chloroform was added. The reaction mixture was stirred for an additional 30 minutes. The two phases were separated and the chloroform phase was washed several times with cool distilled water to remove any inorganic salt. The presence of chloride anions was monitored by silver nitrate test. A rotary evaporator removed the chloroform and an orange wax was obtained in 99.22% yield. 1H and 13C NMR (DMSO) were obtained. Melting point (hot plate apparatus)=30-40° C. Thermal data determined by thermalgravimetric analysis (TGA): Tonset5%=211° C. and Tonset=219° C.

후처리

  1. temperatureby gentle heating
  2. temperatureby gentle heating
  3. stirringstirring
  4. temperaturethe reaction mixture was heated
  5. stirringstirred for 30 minutes
  6. stirringThe reaction mixture was stirred for an additional 30 minutes
  7. customThe two phases were separated
  8. washthe chloroform phase was washed several times
  9. temperaturewith cool
  10. distillationdistilled water
  11. customto remove any inorganic salt
  12. customA rotary evaporator
  13. customremoved the chloroform
  14. customan orange wax was obtained in 99.22% yield
  15. customMelting point (hot plate apparatus)=30-40° C
  16. custom=211° C. and Tonset=219° C.

출처 및 근거

ORD 기록
ord-7c7262f4fc4b4cca9487760f11172ceb
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802596B2

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