Water → Didecyldimethylammonium 2-[(2,6-dichlorophenyl)amino]benzeneacetate

HRID 1517222노트

반응식

HRID 1517222 반응식
[Cl-].[CH2:2]([N+:12]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])([CH3:14])[CH3:13])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].O.[CH:26]1[CH:31]=[C:30]([CH2:32][C:33]([O-:35])=[O:34])[C:29]([NH:36][C:37]2[C:42]([Cl:43])=[CH:41][CH:40]=[CH:39][C:38]=2[Cl:44])=[CH:28][CH:27]=1.[Na+]>C(Cl)(Cl)Cl>[Cl:43][C:42]1[CH:41]=[CH:40][CH:39]=[C:38]([Cl:44])[C:37]=1[NH:36][C:29]1[CH:28]=[CH:27][CH:26]=[CH:31][C:30]=1[CH2:32][C:33]([O-:35])=[O:34].[CH2:15]([N+:12]([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])([CH3:14])[CH3:13])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]

참가 물질

5

반응물 3

HCID 962WaterHCID 23558Didecyldimethylammonium ChlorideHCID 5018304Diclofenac sodium

생성물 1

HCID 69294875Didecyldimethylammonium 2-[(2,6-dichlorophenyl)amino]benzeneacetate수율 100%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Didecyldimethylammonium chloride (0.03 mol) was dissolved in 40 mL distilled water and diclofenac sodium salt (0.04 mol) was added to the solution. The solution was stirred at room temperature for 30 min. Chloroform (40 mL) was added to the reaction mixture and the mixture was stirred. After separation of the phases, the organic phase was washed with 40 mL distilled, cold water until chloride ions were no longer detected using AgNO3. Chloroform was removed and the residue was dried at 50° C. in vacuum. The product, didecyldimethylammonium 2-[(2,6-dichlorophenyl)amino]benzeneacetate (100% yield), was obtained as a grease that is soluble in chloroform, acetone, and DMSO. The product lacks miscibility with water and hexane. Thermogravimetric analysis: Tonset5%=162° C., and Tonset=183° C. 1H and 13C NMR (DMSO) were obtained.

후처리

  1. additionwas added to the solution
  2. stirringthe mixture was stirred
  3. customAfter separation of the phases
  4. washthe organic phase was washed with 40 mL
  5. distillationdistilled
  6. customChloroform was removed
  7. customthe residue was dried at 50° C. in vacuum

출처 및 근거

ORD 기록
ord-037329b8b688443faae99a68f7cf508b
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232265B2

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