Thioglycolic Acid → HCID 178526195、化合物

HRID 2285868ノート

反応式

HRID 2285868 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]([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]

参加物

5

反応物 3

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

生成物 1

HCID 178526195HCID 178526195、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2.0 ml of methylene chloride, 0.03 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%.

後処理

  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

出典と根拠

ORDレコード
ord-08da4de1308c43dea5fc98175f9d5b43
出典データセット
uspto-grants-1982_04
特許番号
US04324741

反応ノート

読み込み中…