Thioglycolic Acid → HCID 178526196, 화합물

HRID 1758185

반응식

HRID 1758185 반응식
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]

참가 물질

5

반응물 3

HCID 1133Thioglycolic AcidHCID 988982,6-Di-tert-butyl-4-methylpyridineHCID 11488264Pentafluoroethylphenyliodonium trifluoromethanesulfonate

생성물 1

HCID 178526196HCID 178526196, 화합물수율 90%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-673309507f5b4cde8c652f74427d1434
출처 데이터셋
uspto-grants-1983_02
특허 번호
US04371710

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