Bromine → 3-Bromo-2-(p-chlorophenyl)-5-[(trifluoromethyl)thio]pyrrole

HRID 129627ノート

反応式

HRID 129627 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][C:10]([S:13][C:14]([F:17])([F:16])[F:15])=[CH:11][CH:12]=2)=[CH:4][CH:3]=1.[Br:18]Br>C(Cl)(Cl)Cl>[Br:18][C:12]1[CH:11]=[C:10]([S:13][C:14]([F:15])([F:17])[F:16])[NH:9][C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 24408BromineHCID 189304232-(p-Chlorophenyl)-5-[(trifluoromethyl)thio]pyrrole

生成物 1

HCID 189304073-Bromo-2-(p-chlorophenyl)-5-[(trifluoromethyl)thio]pyrrole収率 80.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A solution of 2-(p-chlorophenyl)-5-[(trifluoromethyl)thio]pyrrole (1.94 g, 0.00699 mol) in chloroform is cooled, treated with a solution of bromine (1.16 g, 0.00699 mol) in chloroform, stirred for two hours, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a dark syrup. Flash chromatography of the syrup using silica gel and a 1:10 ethyl acetate/hexanes solution gives the title product as a pink syrup (2.0 g) which is identified by 1HNMR and 13CNMR spectral analyses.

後処理

  1. washwashed with water and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated in vacuo
  4. customto obtain a dark syrup

出典と根拠

ORDレコード
ord-68e6dbef26e84b079912465440737c54
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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