Bromine → 5-Bromo-2,3-bis(4-fluorophenyl)thiophene

HRID 280579노트

반응식

HRID 280579 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][CH:10]=[CH:11][C:12]=2[C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.[Br:20]Br>C(Cl)Cl.C(O)(=O)C>[Br:20][C:10]1[S:9][C:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)=[C:12]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[CH:11]=1

참가 물질

5

반응물 2

HCID 24408BromineHCID 119758142,3-Bis(4-fluorophenyl)thiophene

생성물 1

HCID 131272535-Bromo-2,3-bis(4-fluorophenyl)thiophene수율 83.7%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6344Dichloromethane용매

실험 절차

A solution of 2,3-bis(4-fluorophenyl)thiophene (13.6 g, 50 mmole) in 120 ml methylene chloride and 150 ml acetic acid was cooled to ~5° and treated with bromine (2.8 ml, 55 mmole). After 4 hours, the reaction mixture was concentrated in vacuo. The residue was dissolved in ethyl acetate and washed with saturated aqueous sodium bicarbonate and brine, dried and concentrated in vacuo. Recrystallization from ethanol gave the title compound (14.7 g), m.p. 91°-93°.

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with saturated aqueous sodium bicarbonate and brine
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customRecrystallization from ethanol

출처 및 근거

ORD 기록
ord-977e61b7fa6042b49ca1e0a225e3f856
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04590205

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