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Lithium Hydroxide → HCID 21713168、化合物

HRID 650709
ノート
印刷プレビュー

反応式

HRID 650709 の反応式
C[O:2][C:3](=[O:18])/[C:4](/[CH2:15][CH2:16][CH3:17])=[CH:5]/[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7].[OH-].[Li+]>C1COCC1.O>[C:9]1([S:6](/[CH:5]=[C:4](\[CH2:15][CH2:16][CH3:17])/[C:3]([OH:18])=[O:2])(=[O:8])=[O:7])[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 70244124HCID 70244124、化合物

生成物 1

HCID 21713168HCID 21713168、化合物収率 83%

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

(E)-3-benzenesulfonyl-2-propylacrylic acid methyl ester (5.0 g, 16.84 mmol) was dissolved in THF/water 3:1 (20 ml). Lithium hydroxide (0.86 g, 20.49 mmol) was added and the solution was stirred at room temperature overnight. The solvent was evaporated and the mixture was partitioned between ethyl acetate (50 ml) and water (40 ml). The aqueous layer was acidifed with 2M H2SO4 (6 ml) and the product was extracted into ethyl acetate (2×30 ml). The combined organic layers were washed with 2M H2SO4 (20 ml), brine, dried over magnesium sulfate, filtered and evaporated to give the title compound in 83% yield.

後処理

  1. customThe solvent was evaporated
  2. customthe mixture was partitioned between ethyl acetate (50 ml) and water (40 ml)
  3. extractionthe product was extracted into ethyl acetate (2×30 ml)
  4. washThe combined organic layers were washed with 2M H2SO4 (20 ml), brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-697cad24739444a995eb371c53fa8a53
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06274758B1

反応ノート

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