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Ethanol → HCID 21162420、化合物

HRID 894006
ノート
印刷プレビュー

反応式

HRID 894006 の反応式
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[CH:5][C:6]2[S:12][C:11]3[CH:13]=[CH:14][C:15]([CH:17]([CH3:21])[C:18](N)=[O:19])=[CH:16][C:10]=3[C:9](=[O:22])[CH2:8][C:7]=2[CH:23]=1.C([OH:28])C.[OH-].[Na+]>O>[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[CH:5][C:6]2[S:12][C:11]3[CH:13]=[CH:14][C:15]([CH:17]([CH3:21])[C:18]([OH:28])=[O:19])=[CH:16][C:10]=3[C:9](=[O:22])[CH2:8][C:7]=2[CH:23]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 12895877HCID 12895877、化合物

生成物 1

HCID 21162420HCID 21162420、化合物収率 38%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
75 °C

実験手順

To a mixture of 40 mg of 2-(10,11-dihydro-8-trifluoromethyl-11-oxodibenzo[b,f]thiepin-2-yl)-propionamide and 1 ml of ethanol was added 200 mg of sodium hydroxide in 1 ml of water, and the mixture was stirred at 75° C. for 5 hours. After cooling, the solvent or ethanol was removed by distillation to obtain a residue, to which was added water, and the resulting mixture was washed with chloroform. The aqueous layer was acidified with hydrochloric acid and extracted with ethyl acetate. The extract was washed with a saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain a yellow oil, which was thin-layer chromatographed and developed with chloroform-methanol (10:1), thereby obtaining 15 mg (yield: 38%) of 2-(10,11-dihydro-8-trifluoromethyl-11-oxodibenzo[b,f]thiepin-2-yl)-propionic acid as a light yellow oil.

後処理

  1. temperatureAfter cooling
  2. customthe solvent or ethanol was removed by distillation
  3. customto obtain a residue
  4. washthe resulting mixture was washed with chloroform
  5. extractionextracted with ethyl acetate
  6. washThe extract was washed with a saturated sodium chloride solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationThe solvent was distilled off
  9. customto obtain a yellow oil, which
  10. customchromatographed

出典と根拠

ORDレコード
ord-39dc6047fd2d4623ada27d84a6114a3d
出典データセット
uspto-grants-1981_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04282245

反応ノート

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