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Pivalic acid → 2-(4-Fluoro-2-methylphenyl)-6-methoxybenzo[b]thiophene

HRID 632620
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HRID 632620 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH:10]=[CH:9][S:8][C:7]=2[CH:11]=1.Br[C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=1[CH3:20].CC(C)(C)C(O)=O.C([O-])([O-])=O.[K+].[K+]>CC(N(C)C)=O.C(Cl)Cl.O.CC(C1C=C(C(C)C)C(C2C(P(C3CCCCC3)C3CCCCC3)=C(OC)C=CC=2OC)=C(C(C)C)C=1)C.C1C=[C-]C(CCN)=CC=1.Cl[Pd+]>[F:19][C:16]1[CH:17]=[CH:18][C:13]([C:9]2[S:8][C:7]3[CH:11]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]=3[CH:10]=2)=[C:14]([CH3:20])[CH:15]=1
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참가 물질

9

반응물 4

HCID 6417Pivalic acidHCID 11430Potassium CarbonateHCID 967432-Bromo-5-fluorotolueneHCID 136342376-Methoxy-1-benzothiophene

생성물 1

HCID 867306312-(4-Fluoro-2-methylphenyl)-6-methoxybenzo[b]thiophene수율 44%

시약·촉매·용매 4

HCID 25112666
BrettPhos Palladacycle
촉매
HCID 962Water용매
HCID 6344Dichloromethane용매
HCID 31374Dimethylacetamide용매

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온도
150 °C

실험 절차

To a 20 mL microwave vial, 6-methoxybenzo[b]thiophene (1 g, 6.09 mmol), 2-bromo-5-fluorotoluene (0.808 mL, 6.39 mmol), BrettPhos palladacycle(1 st generation) (0.243 g, 0.304 mmol), trimethylacetic acid (1.866 g, 18.27 mmol), and K2CO3 (2.52 g, 18.27 mmol) were suspended in DMA (10 mL). The reaction was heated for 90 min at 150° C. under microwave radiation. The reaction mixture was diluted with DCM and water. The organic layer was collected (phase separator) and concentrated to afford the crude product. The crude material was concentrated onto to silica gel and purified by column chromatography (SiO2, 100% Heptanes) to afford 2-(4-fluoro-2-methylphenyl)-6-methoxybenzo[b]thiophene (730 mg, 2.68 mmol, 44% yield) as a white solid. 1H NMR (400 MHz, CDCL3) δ ppm=7.69 (d, J=9.09 Hz, 1H), 7.43 (dd, J=6.06, 8.59 Hz, 1H), 7.35 (d, J=2.53 Hz, 1H), 7.14 (s, 1H), 7.00-7.10 (m, 2H), 6.90-7.00 (m, 1H), 3.92 (s, 3H), 2.47 (s, 3H).

후처리

  1. customThe organic layer was collected (phase separator)
  2. concentrationconcentrated
  3. customto afford the crude product
  4. concentrationThe crude material was concentrated onto to silica gel
  5. custompurified by column chromatography (SiO2, 100% Heptanes)

출처 및 근거

ORD 기록
ord-42bb359e793e4161a0c6f6b750ad87a5
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321746B2

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