Thioglycolic Acid → HCID 178526195, 화합물

HRID 2285868노트

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HRID 2285868 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]([F:60])([C:56]([F:59])([F:58])[F:57])[C:31]([F:55])([F:54])[C:32]([F:53])([F:52])[C:33]([F:51])([F:50])[C:34]([F:49])([F:48])[C:35]([F:47])([F:46])[C:36]([F:45])([F:44])[I+]C1C=CC=CC=1>C(Cl)Cl>[F:29][C:30]([F:60])([C:56]([F:59])([F:58])[F:57])[C:31]([F:55])([F:54])[C:32]([F:53])([F:52])[C:33]([F:51])([F:50])[C:34]([F:49])([F:48])[C:35]([F:47])([F:46])[C:36]([F:45])([F:44])[CH2:2][C:3]([OH:5])=[S:23]

참가 물질

5

반응물 3

HCID 1133Thioglycolic AcidHCID 988982,6-Di-tert-butyl-4-methylpyridineHCID 2760324(Heptadecafluorooctyl)(phenyl)iodanium trifluoromethanesulfonate

생성물 1

HCID 178526195HCID 178526195, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2.0 ml of methylene chloride, 0.03 ml (0.42 mmol) of mercaptoacetic acid and 80 mg (0.39 mmol) of 2,6-di-tert-butyl-4-methylpyridine were charged in a flask, and 290 mg (0.38 mmol) of heptadecafluoro-n-octylphenyliodonium trifluoromethanesulfonate was added thereto in small portions while stirring at room temperature, followed by stirring for 20 minutes at room temperature. The resulting precipitate was filtered, subjected to silica gel chromatography and, after eluting iodobenzene with pentane, the desired product was eluted with diethyl ether. Diethyl ether was distilled off from the eluate to obtain heptadecafluoro-n-octylthioacetic acid as white crystals. A sample of the product was purified by gas chromatography. Yield, 88%.

후처리

  1. stirringby stirring for 20 minutes at room temperature
  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

출처 및 근거

ORD 기록
ord-08da4de1308c43dea5fc98175f9d5b43
출처 데이터셋
uspto-grants-1982_04
특허 번호
US04324741

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