(+-)-2-Mercaptopropionic acid → HCID 178460598、化合物

HRID 1758182ノート

反応式

HRID 1758182 の反応式
S[CH:2]([CH3:6])[C:3]([OH:5])=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])([CH:2]([CH3:6])[C:3]([OH:5])=[S:24])[C:32]([F:35])([F:34])[F:33]

参加物

5

反応物 3

HCID 62326(+-)-2-Mercaptopropionic acidHCID 988982,6-Di-tert-butyl-4-methylpyridineHCID 11488264Pentafluoroethylphenyliodonium trifluoromethanesulfonate

生成物 1

HCID 178460598HCID 178460598、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2.0 ml of methylene chloride, 0.06 ml (0.68 mmol) of 2-mercaptopropionic acid and 140 mg (0.68 mmol) of 2,6-di-tert-butyl-4-methylpyridine were charged in a flask, and 320 mg (0.68 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 precipitate was filtered, subjected to column chromatography of silica gel and, after eluting iodobenzene with pentane, the desired product was eluted with diethyl ether. Diethyl ether was distilled off from the eluate to obtain 2-pentafluoroethylthiopropionic acid as a colorless liquid. A sample of the product was purified by gas chromatography. Yield, 81%.

後処理

  1. stirringby stirring the mixture at room temperature for 20 minutes
  2. filtrationThe resulting precipitate was filtered
  3. washafter eluting iodobenzene with pentane
  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-d523dfa221194dd9aa091bc17712b4df
出典データセット
uspto-grants-1983_02
特許番号
US04371710

反応ノート

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