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Sodium Hydroxide → (E)-3-[5,6Dimethoxy-3-(4-methoxyphenoxy)benzo[b]thiophen-2-yl]-2-(4-pyridinyl)-2-propenoic acid

HRID 1004118
ノート
印刷プレビュー

反応式

HRID 1004118 の反応式
[CH3:1][O:2][C:3]1[C:33]([O:34][CH3:35])=[CH:32][C:6]2[S:7][C:8](/[CH:19]=[C:20](\[C:26]3[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=3)/[C:21]([O:23]CC)=[O:22])=[C:9]([O:10][C:11]3[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=3)[C:5]=2[CH:4]=1.[OH-].[Na+]>C(O)C>[CH3:1][O:2][C:3]1[C:33]([O:34][CH3:35])=[CH:32][C:6]2[S:7][C:8](/[CH:19]=[C:20](\[C:26]3[CH:27]=[CH:28][N:29]=[CH:30][CH:31]=3)/[C:21]([OH:23])=[O:22])=[C:9]([O:10][C:11]3[CH:12]=[CH:13][C:14]([O:17][CH3:18])=[CH:15][CH:16]=3)[C:5]=2[CH:4]=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 14798Sodium HydroxideHCID 86755303Ethyl (E)-3-[5,6-dimethoxy-3-(4-methoxyphenoxy)benzo[b]thiophen-2-yl]-2-(4-pyridinyl)-2-propenoate

生成物 1

HCID 9912231(E)-3-[5,6Dimethoxy-3-(4-methoxyphenoxy)benzo[b]thiophen-2-yl]-2-(4-pyridinyl)-2-propenoic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution containing 3 mmol of the product of Example 1, 6 ml of an aqueous 1N sodium hydroxide solution and 20 ml of ethanol is refluxed for 2 hours. After returning to room temperature, the reaction mixture is concentrated under reduced pressure and the residue is then diluted in water and subsequently taken up in diethyl ether. The organic phase is then rendered acidic by the addition of 6 ml of a 1N HCl solution. A precipitate forms, which is filtered, rinsed with water and then dried under reduced pressure, enabling 1.3 g of the expected compound to be obtained.

後処理

  1. temperatureis refluxed for 2 hours
  2. customAfter returning to room temperature
  3. concentrationthe reaction mixture is concentrated under reduced pressure
  4. additionthe residue is then diluted in water
  5. additionrendered acidic by the addition of 6 ml of a 1N HCl solution
  6. filtrationA precipitate forms, which is filtered
  7. washrinsed with water
  8. customdried under reduced pressure
  9. customto be obtained

出典と根拠

ORDレコード
ord-3c3fab9e81904ad1b01f910d246bfe71
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06048875

反応ノート

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