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Dichloromethane → 1-methyl-2-(2'-nitrobiphenyl-4-yl)-1H-benzo[d]imidazole

HRID 1509643
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HRID 1509643 반응식
I[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N+:14]([O-:16])=[O:15])=[CH:4][CH:3]=1.[CH3:17][N:18]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[N:20]=[CH:19]1.C(Cl)Cl.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH3:17][N:18]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[N:20]=[C:19]1[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N+:14]([O-:16])=[O:15])=[CH:4][CH:3]=1
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참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 11776TriphenylphosphineHCID 958901H-Benzimidazole, 1-methyl-HCID 6297494'-Iodo-2-nitrobiphenyl

생성물 1

HCID 1181139891-methyl-2-(2'-nitrobiphenyl-4-yl)-1H-benzo[d]imidazole

시약·촉매·용매 1

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매

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온도
65 °C

실험 절차

To a three-necked flask equipped with a magnetic stir bar was added 4′-iodo-2-nitrobiphenyl (3.90 g, 12.0 mmol, 1.2 equiv), 1-methyl-1H-benzo[d]imidazole (1.32 g, 10.0 mmol, 1.0 equiv), Ag2CO3 (5.52 g, 20.0 mmol, 2.0 eq), Pd(dppf)Cl2.CH2Cl2 (0.41 g, 0.5 mmol, 0.05 eq) and PPh3 (0.26 g, 1.0 mmol, 0.1 eq). The tube was evacuated and back-filled with nitrogen, and this evacuation/back-fill procedure was repeated twice. Then solvent CH3CN (60 mL) was added under the protection of nitrogen. The mixture was stirred in an oil bath at a temperature of 60-70° C. for 6.5 days and then cooled. The solid was filtered off through a pad of celite, and washed with ethyl acetate. The filtrate was concentrated under reduced pressure and the residue was purified through column chromatography on silica gel using hexane and ethyl acetate (10:1-5:1-3:1-2:1) as an eluent to afford the desired product, 1-methyl-2-(2′-nitrobiphenyl-4-yl)-1H-benzo[d]imidazole, as a white solid (1.36 g in 41% yield). 1H NMR (DMSO-d6, 400 MHz): δ 3.95 (s, 3H), 7.25-7.29 (m, 1H), 7.31-7035 (m, 1H), 7.57 (d, J=8.0 Hz, 2H), 7.65-7.72 (m, 4H), 7.84 (td, J=7.6, 1.2 Hz, 1H), 7.98 (d, J=7.6 Hz, 2H), 8.06-8.08 (m, 1H).

후처리

  1. customTo a three-necked flask equipped with a magnetic stir bar
  2. customThe tube was evacuated
  3. additionback-filled with nitrogen
  4. additionThen solvent CH3CN (60 mL) was added under the protection of nitrogen
  5. temperaturecooled
  6. filtrationThe solid was filtered off through a pad of celite
  7. washwashed with ethyl acetate
  8. concentrationThe filtrate was concentrated under reduced pressure
  9. customthe residue was purified through column chromatography on silica gel

출처 및 근거

ORD 기록
ord-9f5a1f07d8bd44ffba91080577dbbf36
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09224963B2

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