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Cesium carbonate → Methyl 2-bromo-2',6'-dimethoxybiphenyl-4-carboxylate

HRID 1040353
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HRID 1040353 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1I)[C:5]([O:7][CH3:8])=[O:6].[CH3:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH3:22])[C:16]=1B(O)O.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([C:5]([O:7][CH3:8])=[O:6])[CH:9]=[CH:10][C:11]=1[C:16]1[C:15]([O:14][CH3:13])=[CH:20][CH:19]=[CH:18][C:17]=1[O:21][CH3:22]
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참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 2734343(2,6-Dimethoxyphenyl)boronic acidHCID 17750019Methyl 3-bromo-4-iodobenzoate

생성물 1

HCID 66721235Methyl 2-bromo-2',6'-dimethoxybiphenyl-4-carboxylate수율 56%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매
HCID 6228
Dimethylformamide
용매

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온도
85 °C

실험 절차

Stir a solution of 4.84 g (14.2 mmol) of methyl 3-bromo-4-iodobenzoate (J. Med. Chem., 1999, 42, 4088) and 3.88 g (21.29 mmol) of 2,6-dimethoxyphenyl boronic acid in 120 mL of DMF and 14.2 mL of a 2M aqueous solution of caesium carbonate for 15 minutes under argon, then add 984 mg (0.85 mmol) of Pd(PPh3)4 and heat for 2.5 h at 85° C. After concentration under reduced pressure, distribute the residue obtained in 600 mL of a 1:1 DCM/water mixture. Wash the organic phase with 100 mL of water, dry over MgSO4 and concentrate at reduced pressure. Purify the residue obtained by silica gel column chromatography, eluting with a heptane/EtOAc gradient from 0 to 10% of EtOAc. After concentration under reduced pressure, we obtain 2.79 g of methyl 2-bromo-2′,6′-dimethoxybiphenyl-4-carboxylate in the form of oil.

후처리

  1. concentrationAfter concentration under reduced pressure
  2. customobtained in 600 mL of a 1:1 DCM/water mixture
  3. washWash the organic phase with 100 mL of water
  4. dry with materialdry over MgSO4
  5. concentrationconcentrate at reduced pressure
  6. customPurify the residue
  7. customobtained by silica gel column chromatography
  8. washeluting with a heptane/EtOAc gradient from 0 to 10% of EtOAc
  9. concentrationAfter concentration under reduced pressure, we

출처 및 근거

ORD 기록
ord-28de07a469ee418a9fe2221d0b7db679
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08552201B2

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