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Ethanol → HCID 20295300、化合物

HRID 1389759
ノート
印刷プレビュー

反応式

HRID 1389759 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702Ethanol2 回HCID 20295297HCID 20295297、化合物HCID 23689124Potassium p-toluenesulfonate

生成物 1

HCID 20295300HCID 20295300、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e15781a0e52f4a7dac047e5643d7e3dd
出典データセット
uspto-grants-1981_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04246259

反応ノート

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