Dimethylformamide → N-(3-bromo-6-cyano-2-methoxy-5-methyl-4-styrylphenyl)-2,2-dimethylpropionamide

HRID 17271

반응식

HRID 17271 반응식
CN(C)C=O.[Br:6][C:7]1[C:8]([O:24][CH3:25])=[C:9]([NH:17][C:18](=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20])[C:10]([C:15]#[N:16])=[C:11]([CH3:14])[C:12]=1I.[CH:26](/B(O)O)=[CH:27]\[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>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.C(OCC)(=O)C>[Br:6][C:7]1[C:8]([O:24][CH3:25])=[C:9]([NH:17][C:18](=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20])[C:10]([C:15]#[N:16])=[C:11]([CH3:14])[C:12]=1[CH:26]=[CH:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

참가 물질

6

반응물 3

HCID 6228DimethylformamideHCID 5702628Styrylboronic acidHCID 86630795N-(3-Bromo-6-cyano-4-iodo-2-methoxy-5-methylphenyl)-2,2-dimethylpropionamide

생성물 1

HCID 86630802N-(3-bromo-6-cyano-2-methoxy-5-methyl-4-styrylphenyl)-2,2-dimethylpropionamide

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 8857Ethyl Acetate용매

반응 조건

온도
95 °C

실험 절차

Tetrakis(triphenylphosphine)palladium(0) (6.4 mg, 5.5 μmol) was added to an N,N-dimethylformamide (1.0 ml) suspension of N-(3-bromo-6-cyano-4-iodo-2-methoxy-5-methylphenyl)-2,2-dimethylpropionamide (I-6) (50 mg, 111 μmol), trans-β-styreneboronic acid (17.2 mg, 116 μmol), potassium phosphate n-hydrate (74-78%, 64 mg, 222 μmol), followed by stirred overnight at 95° C. The reaction liquid was cooled, then ethyl acetate (30 ml) was added, followed by washing with saturated brine (30 ml×2), drying over anhydrous magnesium sulfate, concentrating under reduced pressure.

후처리

  1. customThe reaction liquid
  2. temperaturewas cooled
  3. washby washing with saturated brine (30 ml×2)
  4. dry with materialdrying over anhydrous magnesium sulfate
  5. concentrationconcentrating under reduced pressure

출처 및 근거

ORD 기록
ord-be1549dc55c14a9f9e3975d546dc35d8
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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