4-Chlorobenzenesulfonyl chloride → 2,2,2-Trifluoroethane-1-sulfonamide

HRID 853774ノート

反応式

HRID 853774 の反応式
[F:1][C:2]([F:11])([F:10])[CH2:3]N1CCCCC1.C([N:14](CC)CC)C.ClC1C=CC([S:26](Cl)(=[O:28])=[O:27])=CC=1>ClCCCl>[F:1][C:2]([F:11])([F:10])[CH2:3][S:26]([NH2:14])(=[O:28])=[O:27]

参加物

5

反応物 3

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 8471TriethylamineHCID 178400041-(2,2,2-Trifluoroethyl)piperidine

生成物 1

HCID 212655462,2,2-Trifluoroethane-1-sulfonamide収率 114.1%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

To a solution of O-protected trifluoroethyl piperidine (1.13 g, 3.6 mmol) in DCE (15 mL) was added triethylamine (0.6 mL, 4.3 mmol) then 4-chlorobenzenesulfonyl chloride (1.13 g, 5.4 mmol) and the reaction mixture was heated at reflux overnight. The final mixture was concentrated and directly purified by flash chromatography over silica gel (eluting with hexane to DCM) to afford 0.67 g (38%) of O-protected trifluoroethyl sulfonamide.

後処理

  1. temperatureat reflux overnight
  2. concentrationThe final mixture was concentrated
  3. customdirectly purified by flash chromatography over silica gel (eluting with hexane to DCM)

出典と根拠

ORDレコード
ord-6f48be7f0b274a12b71403a5aec730ef
出典データセット
uspto-grants-2007_08
特許番号
US07256186B2

反応ノート

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