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

HRID 234313

반응식

HRID 234313 반응식
[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

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 681202,2'-Bithiophene

생성물 1

HCID 6400655-Bromo-[2,2']bithiophenyl수율 88.2%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7caf47112e3549159a68279fb777c113
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594021

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