3-Mercaptopropionic Acid → HCID 178526190、化合物

HRID 1758183

反応式

HRID 1758183 の反応式
S[CH2:2][CH2:3][C:4]([OH:6])=O.C(C1C=C(C)C=C(C(C)(C)C)N=1)(C)(C)C.FC(F)(F)[S:24]([O-])(=O)=O.[F:30][C:31]([I+]C1C=CC=CC=1)([F:36])[C:32]([F:35])([F:34])[F:33]>C(Cl)Cl>[F:30][C:31]([F:36])([CH2:2][CH2:3][C:4]([OH:6])=[S:24])[C:32]([F:35])([F:34])[F:33]

参加物

5

実験手順

2.0 ml of methylene chloride, 0.05 ml (0.58 mmol) of 3-mercaptopropionic acid and 120 mg (0.59 mmol) of 2,6-di-tert-butyl-4-methylpyridine were charged in a flask, and 261 mg (0.55 mmol) of pentafluoroethylphenyliodonium trifluoromethanesulfonate was added thereto in small portions while stirring at room temperature, followed by stirring the mixture at room temperature for 20 minutes. The resulting white precipitate was filtered, subjected to column chromatography of a small amount of silica gel and, after eluting iodobenzene with hexane, the desired product was eluted with diethyl ether. Diethyl ether was distilled off from the eluate to obtain 3-pentafluoroethylthiopropionic acid as a colorless liquid. A sample of the product was purified by gas chromatography. Yield, 83%.

後処理

  1. stirringby stirring the mixture at room temperature for 20 minutes
  2. filtrationThe resulting white precipitate was filtered
  3. washafter eluting iodobenzene with hexane
  4. washthe desired product was eluted with diethyl ether
  5. distillationDiethyl ether was distilled off from the eluate

出典と根拠

ORDレコード
ord-071eaa1c832b47528a922645f141246c
出典データセット
uspto-grants-1983_02
特許番号
US04371710

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