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Ethanol → HCID 20572291、化合物

HRID 1577309
ノート
印刷プレビュー

反応式

HRID 1577309 の反応式
F[B-](F)(F)F.[C:6]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[S+:17]([CH2:36][CH2:37][CH3:38])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])([O:8][CH2:9][CH3:10])=[O:7].C(O)C.[S:42]([C:46]1[CH:52]=[CH:51][C:49]([CH3:50])=[CH:48][CH:47]=1)([O-:45])(=[O:44])=[O:43].[K+].O>C(Cl)Cl>[C:49]1([CH3:50])[CH:48]=[CH:47][C:46]([S:42]([O-:45])(=[O:43])=[O:44])=[CH:52][CH:51]=1.[C:6]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[S+:17]([CH2:36][CH2:37][CH3:38])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])([O:8][CH2:9][CH3:10])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702Ethanol2 回HCID 962WaterHCID 12760768HCID 12760768、化合物HCID 23689124Potassium p-toluenesulfonate

生成物 1

HCID 20572291HCID 20572291、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5.0 g of o-carbethoxyphenyl-n-propyl-n-octadecylsulfonium tetrafluoroborate in 20 ml. of ethanol is added 20.0 g of potassium tosylate 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 filtered, and the filtrate then evaporated under vacuum to dryness to obtain a residue. The residue is taken up in methylene chloride; the organic phase washed several times with water, dried over sodium sulphate, filtered and evaporated under vacuum to dryness. The residue is chromatographed over silica gel three times using methylene chloride and increasing amounts of methanol to obtain the title product m.p. 65°-67°.

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. filtrationfiltered
  5. customthe filtrate then evaporated under vacuum to dryness
  6. customto obtain a residue
  7. washthe organic phase washed several times with water
  8. dry with materialdried over sodium sulphate
  9. filtrationfiltered
  10. customevaporated under vacuum to dryness
  11. customThe residue is chromatographed over silica gel three times
  12. temperatureincreasing amounts of methanol

出典と根拠

ORDレコード
ord-d9874629d29d482cb198e38ecbffd9c6
出典データセット
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04287355

反応ノート

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