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Sodium Hydroxide → 2-(2-(1-Benzothiophene-5-yl)ethoxy)acetic acid

HRID 1007926
ノート
印刷プレビュー

反応式

HRID 1007926 の反応式
[S:1]1[CH:5]=[CH:4][C:3]2[CH:6]=[C:7]([CH2:10][CH2:11][O:12][CH2:13][C:14](N3CCCCC3)=[O:15])[CH:8]=[CH:9][C:2]1=2.[OH-:22].[Na+]>C(O)C.O>[S:1]1[CH:5]=[CH:4][C:3]2[CH:6]=[C:7]([CH2:10][CH2:11][O:12][CH2:13][C:14]([OH:15])=[O:22])[CH:8]=[CH:9][C:2]1=2
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 2

HCID 14798Sodium HydroxideHCID 226663742-(2-Benzo[b]thiophen-5-ylethoxy)-1-piperidino-1-ethanone

生成物 1

HCID 219900582-(2-(1-Benzothiophene-5-yl)ethoxy)acetic acid収率 74.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

In a mixture of 58 mL of ethanol and 6 mL of water is dissolved 6.40 g of 2-(2-benzo[b]thiophen-5-ylethoxy)-1-piperidino-1-ethanone, to which is added 1.27 g of sodium hydroxide. The mixture is heated under reflux for 4 hours. After cooling the mixture, the deposited matter is collected by filtration. The deposited matter is added to a mixture of ethyl acetate and water, pH is adjusted to 1.5 with 2 mol/L hydrochloric acid, and the organic layer is separated. The organic layer is washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure to obtain 3.72 g of 2-(2-benzo[b]thiophen-5-ylethoxy)-acetic acid as a colorless crystalline product.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 4 hours
  3. temperatureAfter cooling the mixture
  4. filtrationthe deposited matter is collected by filtration
  5. additionThe deposited matter is added to a mixture of ethyl acetate and water, pH
  6. customthe organic layer is separated
  7. washThe organic layer is washed with water and saturated aqueous solution of sodium chloride
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-0b252585547a46fe8a2240492bf34990
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06797726B1

反応ノート

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