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Toluene → 3'-Methoxybiphenyl-3-carboxylic acid amide

HRID 347668
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HRID 347668 반응식
Br[C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([NH2:7])=[O:6].C1(C)C=CC=CC=1.C([O-])([O-])=O.[Na+].[Na+].[CH3:24][O:25][C:26]1[CH:27]=[C:28](B(O)O)[CH:29]=[CH:30][CH:31]=1>O.CCO.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>[CH3:24][O:25][C:26]1[CH:31]=[C:30]([C:2]2[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([NH2:7])=[O:6])[CH:3]=2)[CH:29]=[CH:28][CH:27]=1
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참가 물질

8

반응물 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 898073-BromobenzamideHCID 2734370(3-Methoxyphenyl)boronic acid

생성물 1

HCID 671227163'-Methoxybiphenyl-3-carboxylic acid amide수율 74.1%

시약·촉매·용매 3

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 702Ethanol용매
HCID 962Water용매

실험 절차

To a stirred mixture 3-bromobenzoic acid amide (0.76 g; 3.8 mmol) and toluene (25 mL), Pd(PPh3)4 (0.180 g; 0.16 mmol), a solution of Na2CO3 (2.543 g; 24 mmol) in H2O (10 mL), and one of 3-methoxyphenylboronic acid (1.132 g; 7.45 mmol) in EtOH (10 mL) were added. The mixture was refluxed for 1 h under vigorous stirring, cooled, and the acqueous phase extracted with AcOEt. The combined organic layers were dried over Na2SO4 and concentrated. Purification of the residue by column chromatography (cyclohexane/EtOAc 1:1 then 4:6) and recrystallization gave the desired product (0.64 g) as white solid. Yield 74%. Mp: 138–40° C. (EtOH). MS (EI): m/z 227 (M+, 100%). 1H NMR (CDCl3): δ 3.88 (s, 3H); 5.71 (br s, 1H); 6.11 (br s, 1H); 6.94 (m, 1H); 7.18 (m, 2H); 7.39 (t, 1H); 7.53 (t, 1H); 7.77 (m, 2H); 8.05 (t, 1H) ppm. IR (Nujol): 3327, 3148, 1676, 1640, 1613, 1584 cm−1.

후처리

  1. temperatureThe mixture was refluxed for 1 h under vigorous stirring
  2. temperaturecooled
  3. extractionthe acqueous phase extracted with AcOEt
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. concentrationconcentrated
  6. customPurification of the residue by column chromatography (cyclohexane/EtOAc 1:1
  7. custom4:6) and recrystallization

출처 및 근거

ORD 기록
ord-ed744bcc679f47c18f6717b83fd60aaf
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07176201B2

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