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Ethanol → HCID 20295300, 화합물

HRID 1389759
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HRID 1389759 반응식
F[B-](F)(F)F.[C:6]1([S+:12]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(O)C.[S:40]([C:44]1[CH:50]=[CH:49][C:47]([CH3:48])=[CH:46][CH:45]=1)([O-:43])(=[O:42])=[O:41].[K+]>O>[C:47]1([CH3:48])[CH:46]=[CH:45][C:44]([S:40]([O-:43])(=[O:41])=[O:42])=[CH:50][CH:49]=1.[CH2:13]([S+:12]([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702Ethanol2회HCID 20295297HCID 20295297, 화합물HCID 23689124Potassium p-toluenesulfonate

생성물 1

HCID 20295300HCID 20295300, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 5.0 g diphenyl-n-octadecyl sulfonium tetrafluoroborate in 20 ml. of ethanol is added 20.0 g of potassiumtosylate dissolved in a mixture of 200 ml. ethanol and 10 ml. water. The reaction mixture is maintained at 80°-90° while being stirred vigorously for 2 hours. The reaction mixture is then cooled and evaporated i.v. to dryness. The residue is taken up in methylene chloride; the organic phase washed several times with water, dried over sodium sulphate, filtered and evaporated i.v. to dryness. The residue is chromatographed over silica gel three times using methylene chloride and increasing amounts of methanol to obtain n-octadecyldiphenylsulfonium p-toluenesulfonate.

후처리

  1. dissolutiondissolved in a mixture of 200 ml
  2. temperatureThe reaction mixture is maintained at 80°-90°
  3. temperatureThe reaction mixture is then cooled
  4. customevaporated i.v
  5. washthe organic phase washed several times with water
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated i.v
  9. customThe residue is chromatographed over silica gel three times
  10. temperatureincreasing amounts of methanol

출처 및 근거

ORD 기록
ord-e15781a0e52f4a7dac047e5643d7e3dd
출처 데이터셋
uspto-grants-1981_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04246259

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