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Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 71246625、化合物

HRID 1620764
ノート
印刷プレビュー

反応式

HRID 1620764 の反応式
[OH:1][C:2]1([C@H:5]2[CH2:9][O:8]C(C)(C)[N:6]2[C:12]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[O:13])[CH2:4][CH2:3]1.CC1C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.C(=O)([O-])O.[Na+]>CO>[CH2:15]([O:14][C:12](=[O:13])[NH:6][C@@H:5]([C:2]1([OH:1])[CH2:3][CH2:4]1)[CH2:9][OH:8])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
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 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 516892Sodium BicarbonateHCID 11460510HCID 11460510、化合物

生成物 1

HCID 71246625HCID 71246625、化合物収率 79.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of benzyl(4R)-4-(1-hydroxycyclopropyl)-2,2-dimethyl-1,3-oxazolidine-3-carboxylate (2.45 g) in methanol (100 mL) was added pyridin-1-ium 4-methylbenzenesulfonate (2.33 g) at room temperature. The reaction mixture was stirred at room temperature overnight, to the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was separated, washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.68 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe organic layer was separated
  3. washwashed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-085e1b5cc91a43919c98b6befa203090
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772277B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート