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1-Pentanol → Triphenylsulfonium 2,4,6-triisopropylbenzoate

HRID 529865
ノート
印刷プレビュー

反応式

HRID 529865 の反応式
[CH:1]([C:4]1[CH:12]=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:10]=[C:9]([CH:16]([CH3:18])[CH3:17])[C:5]=1[C:6]([O-:8])=[O:7])([CH3:3])[CH3:2].[Na+].COS([O-])(=O)=O.[C:26]1([S+:32]([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.C(C(C)=O)(C)C.C(O)CCCC>O>[CH:1]([C:4]1[CH:12]=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:10]=[C:9]([CH:16]([CH3:18])[CH3:17])[C:5]=1[C:6]([O-:8])=[O:7])([CH3:3])[CH3:2].[C:39]1([S+:32]([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=1
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 62761-PentanolHCID 112513-Methyl-2-butanoneHCID 22995011Triphenylsulfonium methylsulfateHCID 118556701Sodium 2,4,6-triisopropylbenzoate

生成物 1

HCID 131735631Triphenylsulfonium 2,4,6-triisopropylbenzoate収率 80%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

A 1-L eggplant shaped flask was charged with 22.4 g of sodium 2,4,6-triisopropylbenzoate (prepared in Synthesis Example 1-2), 31.1 g of triphenylsulfonium methylsulfate, 90 g of methyl isopropyl ketone, 90 g of 1-pentanol, and 40 g of water, which were stirred at room temperature for 1 hour. The organic layer was separated from the reaction mixture and washed with water. After washing, the organic layer was concentrated by distilling off the solvent. The liquid concentrate was crystallized from 300 g of diisopropyl ether. The crystal precipitate was filtered and dried, obtaining the target compound, triphenylsulfonium 2,4,6-triisopropylbenzoate as white crystal. Amount 40.4 g, yield 80%.

後処理

  1. customThe organic layer was separated from the reaction mixture
  2. washwashed with water
  3. washAfter washing
  4. concentrationthe organic layer was concentrated
  5. distillationby distilling off the solvent
  6. concentrationThe liquid concentrate
  7. customwas crystallized from 300 g of diisopropyl ether
  8. filtrationThe crystal precipitate was filtered
  9. customdried

出典と根拠

ORDレコード
ord-c896c67c342f48fa8f84747cf3535aa3
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09348227B2

反応ノート

読み込み中…

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