Water → 4-(1,3-Dithian-2-ylidene)-4-(4-phenoxyphenyl)butyric acid

HRID 2372429

反応式

HRID 2372429 の反応式
[S:1]1[CH2:6][CH2:5][CH2:4][S:3][C:2]1=[C:7]([C:14]1[CH:19]=[CH:18][C:17]([O:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[CH:16][CH:15]=1)[CH2:8][CH2:9][C:10]([O:12]C)=[O:11].O>O1CCCC1.C(O)C.[OH-].[Na+]>[S:1]1[CH2:6][CH2:5][CH2:4][S:3][C:2]1=[C:7]([C:14]1[CH:19]=[CH:18][C:17]([O:20][C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)=[CH:16][CH:15]=1)[CH2:8][CH2:9][C:10]([OH:12])=[O:11]

参加物

6

反応物 2

HCID 962WaterHCID 14674064Methyl 4-(1,3-dithian-2-ylidene)-4-(4-phenoxyphenyl)-butyrate

生成物 1

HCID 146740664-(1,3-Dithian-2-ylidene)-4-(4-phenoxyphenyl)butyric acid収率 97%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

Methyl 4-(1,3-dithian-2-ylidene)-4-(4-phenoxyphenyl)-butyrate, 1.29 g, was dissolved in a solvent mixture of 30 ml of tetrahydrofuran and 30 ml of ethanol and, 10 ml of 1 N sodium hydroxide aqueous solution was added to the solution followed by stirring at room temperature for 2 hours. Water was added to the reaction mixture. After washing with ethyl acetate, the aqueous phase was rendered acidic with conc. hydrochloric acid and extracted with ethyl acetate. After drying the ethyl acetate phase over magnesium sulfate, the solvent was distilled off under reduced pressure and the residue was crystallized from ether to give 1.21 g of white crystals.

後処理

  1. additionwas added to the solution
  2. washAfter washing with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. dry with materialAfter drying the ethyl acetate phase over magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customthe residue was crystallized from ether

出典と根拠

ORDレコード
ord-4b39fa1ceb65491daa2194fd5748cf0a
出典データセット
uspto-grants-1992_03
特許番号
US05098928

関連ノート

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