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Sodium Bicarbonate → 2-(4-hydroxybutyloxy)acetic Acid Tert-Butyl Ester

HRID 1271249
ノート
印刷プレビュー

反応式

HRID 1271249 の反応式
[C:1]([O:5][C:6](=[O:20])[CH2:7][O:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13]C1CCCCO1)([CH3:4])([CH3:3])[CH3:2].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)([O-])O.[Na+]>CO>[C:1]([O:5][C:6](=[O:20])[CH2:7][O:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13])([CH3:4])([CH3:2])[CH3:3]
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 516892Sodium BicarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 693544612-[4-(2-tetrahydropyranyloxy)butyloxy]acetic Acid Tert-Butyl Ester

生成物 1

HCID 865924582-(4-hydroxybutyloxy)acetic Acid Tert-Butyl Ester収率 66.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 36.21 g of 2-[4-(2-tetrahydropyranyloxy)butyloxy]acetic acid tert-butyl ester in 360 ml of methanol, 47.77 g of p-toluenesulfonic acid monohydrate was added. After stirring at room temperature for 30 minutes, the reaction solution was neutralized with an aqueous sodium hydrogen carbonate solution and the solvent was evaporated under reduced pressure. The residue was diluted with water, extracted with diethyl ether, washed with water and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 17.02 g of the desired compound as a colorless oily substance.

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. additionThe residue was diluted with water
  3. extractionextracted with diethyl ether
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-388b95db04074cf08e2086b9ced83f2a
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07205302B2

反応ノート

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