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Potassium Hydroxide → HCID 68642113, 화합물

HRID 1498947
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HRID 1498947 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 9344223HCID 9344223, 화합물HCID 12217721Iodo benzene diacetate

생성물 1

HCID 68642113HCID 68642113, 화합물수율 26.7%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-d6869d1da192415f8c5108dc5483b6d5
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200008B2

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