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Potassium Hydroxide → HCID 68642113、化合物

HRID 1498947
ノート
印刷プレビュー

反応式

HRID 1498947 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[S:10][C:11]([C:15](=[O:17])[CH3:16])=[C:12]([CH3:14])[N:13]=1.[OH-:18].[K+].[C:20](O)(=[O:22])C.[C:24](O)(=O)C.IC1C=CC=CC=1>CO>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[S:10][C:11]([C:15]([O:22][CH3:20])([O:17][CH3:24])[CH2:16][OH:18])=[C:12]([CH3:14])[N:13]=1
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 3

HCID 14797Potassium HydroxideHCID 9344223HCID 9344223、化合物HCID 12217721Iodo benzene diacetate

生成物 1

HCID 68642113HCID 68642113、化合物収率 26.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To methanol (5 ml), 1-[2-(2,4-dimethylphenyl)-4-methylthiazol-5-yl]ethanone (981 mg) prepared in the Step 31-1-1 was added, and a solution of potassium hydroxide (673 mg) in methanol (10 ml) was added dropwise thereto under cooling by ice and stirring. Thereafter, iodobenzene diacetate (1.42 g) was added to the mixture, and then the resulting mixture was stirred at a room temperature for 22 hours. From the mixture methanol was distilled off under a reduced pressure, and water was added to the residue. The resulting mixture was subjected to extraction with dichloromethane. The extract was dried over anhydrous sodium sulfate, and then dichloromethane was distilled off under a reduced pressure. Hexane was added to the residue, the precipitate was separated by filtration, washed with hexane, and then dried under a reduced pressure to give the title compound (328 mg, 26%).

後処理

  1. additionwas added
  2. temperatureunder cooling by ice
  3. stirringthe resulting mixture was stirred at a room temperature for 22 hours
  4. distillationFrom the mixture methanol was distilled off under a reduced pressure, and water
  5. additionwas added to the residue
  6. extractionThe resulting mixture was subjected to extraction with dichloromethane
  7. dry with materialThe extract was dried over anhydrous sodium sulfate
  8. distillationdichloromethane was distilled off under a reduced pressure
  9. additionHexane was added to the residue
  10. customthe precipitate was separated by filtration
  11. washwashed with hexane
  12. customdried under a reduced pressure

出典と根拠

ORDレコード
ord-d6869d1da192415f8c5108dc5483b6d5
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09200008B2

反応ノート

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