1-Dodecanethiol → 1-Pentafluoroethylthiododecane

HRID 1758184ノート

反応式

HRID 1758184 の反応式
[CH2:1]([SH:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C(C1C=C(C)C=C(C(C)(C)C)N=1)(C)(C)C.FC(F)(F)S([O-])(=O)=O.[F:37][C:38]([I+]C1C=CC=CC=1)([F:43])[C:39]([F:42])([F:41])[F:40]>C(Cl)Cl>[F:37][C:38]([F:43])([S:13][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:39]([F:42])([F:41])[F:40]

参加物

5

反応物 3

HCID 81951-DodecanethiolHCID 988982,6-Di-tert-butyl-4-methylpyridineHCID 11488264Pentafluoroethylphenyliodonium trifluoromethanesulfonate

生成物 1

HCID 128906271-Pentafluoroethylthiododecane

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2.0 ml of methylene chloride, 0.10 ml (0.42 mmol) of 1-dodecanethiol and 87 mg (0.42 mmol) of 2,6-di-tert-butyl-4-methylpyridine were added to a flask, and 198 mg (0.42 mmol) of pentafluoroethylphenyliodonium trifluoromethanesulfonate was added thereto in small portions while stirring at room temperature, followed by stirring at room temperature for 20 minutes. The resulting white precipitate was filtered and subjected to column chromatography of silica gel. Iodobenzene and the product were eluted with pentane and purified by gas chromatography to obtain 1-pentafluoroethylthiododecane as an oily substance. Yield, 87%.

後処理

  1. stirringby stirring at room temperature for 20 minutes
  2. filtrationThe resulting white precipitate was filtered
  3. washIodobenzene and the product were eluted with pentane
  4. custompurified by gas chromatography

出典と根拠

ORDレコード
ord-79163db0c8f444d69b79b8419bf7bd58
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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