Thioglycolic Acid → HCID 178526196、化合物

HRID 1758185

反応式

HRID 1758185 の反応式
S[CH2:2][C:3]([OH:5])=O.C(C1C=C(C)C=C(C(C)(C)C)N=1)(C)(C)C.FC(F)(F)[S:23]([O-])(=O)=O.[F:29][C:30]([I+]C1C=CC=CC=1)([F:35])[C:31]([F:34])([F:33])[F:32]>C(Cl)Cl>[F:29][C:30]([CH2:2][C:3]([OH:5])=[S:23])([F:35])[C:31]([F:34])([F:33])[F:32]

参加物

5

実験手順

0.12 ml of mercaptoacetic acid and 350 ml of 2,6-di-tert-butyl-4-methylpyridine were added to 4 ml of methylene chloride and the mixture was stirred at room temperature. Then, 800 mg of pentafluoroethylphenyliodonium trifluoromethanesulfonate was added thereto and the mixture was allowed to react for 30 minutes at room temperature. The reaction mixture was subjected to column chromatography of silica gel and, after eluting iodobenzene with hexane, the product was eluted with diethyl ether. The diethyl ether was distilled off to obtain 319 mg (90% yield) of pentafluoroethylthioacetic acid as an oily substance. 19F-NMR (CCl3F internal standard in CDCl3): -83.98 ppm (t, JCF3,CF2 =3.5 Hz, CF3), -93.39 ppm (q, JCF3,CF2 =3.5 Hz, CF2)

後処理

  1. customto react for 30 minutes at room temperature
  2. washafter eluting iodobenzene with hexane
  3. washthe product was eluted with diethyl ether
  4. distillationThe diethyl ether was distilled off

出典と根拠

ORDレコード
ord-673309507f5b4cde8c652f74427d1434
出典データセット
uspto-grants-1983_02
特許番号
US04371710

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