N-bromobutanimide → 5-Bromo-[2,2']bithiophenyl

HRID 232747

反応式

HRID 232747 の反応式
[Br:1]N1C(=O)CCC1=O.[S:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[C:14]1[S:15][CH:16]=[CH:17][CH:18]=1>C(O)(=O)C.C(Cl)(Cl)Cl>[Br:1][C:13]1[S:9][C:10]([C:14]2[S:15][CH:16]=[CH:17][CH:18]=2)=[CH:11][CH:12]=1

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 681202,2'-Bithiophene

生成物 1

HCID 6400655-Bromo-[2,2']bithiophenyl収率 88.2%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 6212Chloroform溶媒

実験手順

N-bromosuccinimide (NBS, 1.12 g, 6.3 mmol) was added in small portions to a stirred solution of 1.0 g (6.01 mmol) of 2,2'-bithiophene in 10 ml of glacial acetic acid and 10 ml of chloroform. After stirring for 1 h at room temperature, the mixture was poured into ice-water and extracted into chloroform (75 ml). The organic layer was washed with aqueous sodium bicarbonate solution, water, and then dried over magnesium sulfate and evaporated. The residue was subjected to flash chromatography on silica gel using hexane to give 1.3 g (88%) of a light green solid, m.p. 55°-56° C.

後処理

  1. extractionextracted into chloroform (75 ml)
  2. washThe organic layer was washed with aqueous sodium bicarbonate solution, water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-0c9b7ec28b394c7688e607a6c82f74df
出典データセット
uspto-grants-1997_01
特許番号
US05591761

関連ノート

読み込み中…