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Ethyl Acetate → HCID 59296133, 화합물

HRID 2233552
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HRID 2233552 반응식
[F:1][S:2]([F:15])([F:14])([F:13])([F:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH2:9])=[S:8])=[CH:5][CH:4]=1.[CH3:16][O:17][C:18](=[O:25])[CH2:19][C:20](=O)[CH:21](Br)[CH3:22].[CH2:26](OC(=O)C)C>CC(C)=O>[CH2:16]([O:17][C:18](=[O:25])[CH2:19][C:20]1[N:9]=[C:7]([C:6]2[CH:5]=[CH:4][C:3]([S:2]([F:12])([F:13])([F:14])([F:15])[F:1])=[CH:11][CH:10]=2)[S:8][C:21]=1[CH3:22])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 9815681Methyl 4-bromo-3-oxopentanoateHCID 59296136(OC-6-21)-[4-(Aminothioxomethyl)phenyl]pentafluorosulfur

생성물 1

HCID 59296133HCID 59296133, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

0 g 4-Pentafluorosulfanyl-thiobenzamide and 9.93 g 4-bromo-3-oxo-pentanoic acid methyl ester were dissolved in 30 ml acetone and refluxed for one hour. The cooled reaction mixture was diluted by adding 250 ml ethylacetate and washed three times with saturated NaHCO3 solution. The organic layer was dried over MgSO4 and the solvent was removed in vacuo. The residue was purified by flash chromatography with the eluent n-heptane:ethyl acetate=5:1 to provide 4.5 g [5-Methyl-2-(4-pentafluorosulfanyl-phenyl)-thiazol-4-yl]-acetic acid ethyl ester as an oil which solidified upon standing.

후처리

  1. temperaturerefluxed for one hour
  2. customThe cooled reaction mixture
  3. additionwas diluted
  4. washwashed three times with saturated NaHCO3 solution
  5. dry with materialThe organic layer was dried over MgSO4
  6. customthe solvent was removed in vacuo
  7. customThe residue was purified by flash chromatography with the eluent n-heptane

출처 및 근거

ORD 기록
ord-700f0d0a9bcb4b5783a2c32746f10ecd
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07709509B2

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