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Ethyl Acetate → HCID 59296133、化合物

HRID 2233552
ノート
印刷プレビュー

反応式

HRID 2233552 の反応式
[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]
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 8857Ethyl AcetateHCID 9815681Methyl 4-bromo-3-oxopentanoateHCID 59296136(OC-6-21)-[4-(Aminothioxomethyl)phenyl]pentafluorosulfur

生成物 1

HCID 59296133HCID 59296133、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-700f0d0a9bcb4b5783a2c32746f10ecd
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709509B2

反応ノート

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