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Water → HCID 19366807、化合物

HRID 849532
ノート
印刷プレビュー

反応式

HRID 849532 の反応式
C[CH:2]([CH:6]([S:8]([C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1)(=[O:10])=[O:9])[CH3:7])[C:3](O)=[O:4].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[CH3:18][O:17][C:14]1[CH:13]=[CH:12][C:11]([S:8]([CH:6]([CH3:7])[CH2:2][CH2:3][OH:4])(=[O:9])=[O:10])=[CH:16][CH:15]=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 962Water2 回HCID 14798Sodium HydroxideHCID 19366821HCID 19366821、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 19366807HCID 19366807、化合物収率 85%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Part B: To a solution of 3.5 g (13 mmol) of methyl 3-[(4-methoxyphenyl)sulfonyl]-butanoic acid from Part A in 50 mL of anhydrous THF at zero° C. under nitrogen, was added 14.2 mL (0.5 g, 13 mmol) of a 1.0 M solution of lithium aluminum hydride in THF. After 1.5 hours, the reaction mixture was cooled to zero° C. and z0.6 mL of water was added, followed by 0.6 mL of 2.5 N sodium hydroxide solution and 1.8 mL of water, the reaction was filtered, the filtrate concentrated in vacuo, ethyl acetate and 5% citric acid solution were added, the organic layer was separated and washed with saturated sodium bicarbonate solution and brine, dried with magnesium sulfate, filtered and concentrated to afford 2.7 grams of pure 3-[(4-methoxyphenyl)-sulfonyl]butan-1-ol, m/z=251 (M+Li).

後処理

  1. temperaturethe reaction mixture was cooled
  2. filtrationthe reaction was filtered
  3. concentrationthe filtrate concentrated in vacuo, ethyl acetate and 5% citric acid solution
  4. additionwere added
  5. customthe organic layer was separated
  6. washwashed with saturated sodium bicarbonate solution and brine
  7. dry with materialdried with magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-88a3cef68c2f43c9bb72c62c3f7c77a9
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06013649

反応ノート

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