Sodium Carbonate → 2-(p-Chlorophenyl)-5-[(trifluoromethyl)thio]pyrrole

HRID 129626ノート

反応式

HRID 129626 の反応式
[F:1][C:2]([F:6])([F:5])[S:3]Cl.[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[NH:15][CH:16]=[CH:17][CH:18]=2)=[CH:10][CH:9]=1.C(=O)([O-])[O-].[Na+].[Na+]>CCOCC.O.CCOCC>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]([C:14]2[NH:15][C:16]([S:3][C:2]([F:6])([F:5])[F:1])=[CH:17][CH:18]=2)=[CH:12][CH:13]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 67900Methanesulfenyl chloride, trifluoro-HCID 2724282-(4-Chlorophenyl)-1h-pyrrole

生成物 1

HCID 189304232-(p-Chlorophenyl)-5-[(trifluoromethyl)thio]pyrrole

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 21584184Diethylether water溶媒

実験手順

Trifluoromethylsulfenyl chloride is bubbled into a solution of 2-(p-chlorophenyl)pyrrole (0.5 g, 0.00281 mol) and sodium carbonate (0.36 g, 0.00338 mol) in ether at -30° C. under nitrogen. The reaction mixture is stirred for 1/2 hour and diluted with a water/ether mixture. The organic phase is separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title product as a purple solid (0.78 g, mp 34°-39° C.) which is identified by 1HNMR and 13CNMR spectral analyses.

後処理

  1. customThe organic phase is separated
  2. washwashed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e5932f01af404e01bc526dd5290de688
出典データセット
uspto-grants-1995_11
特許番号
US05468877

反応ノート

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