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Dimethylformamide → methyl 1-(4-chlorobenzyl)-4-phenyl-1H-pyrrole-2-carboxylate

HRID 1909887
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HRID 1909887 반응식
Br[C:2]1[CH:3]=[C:4]([C:15]([O:17][CH3:18])=[O:16])[N:5]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[CH:6]=1.CN(C=O)C.[C:24]1(OB(O)O)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(=O)([O-])[O-].[Na+].[Na+]>[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O.C(OCC)(=O)C>[Cl:14][C:11]1[CH:12]=[CH:13][C:8]([CH2:7][N:5]2[CH:6]=[C:2]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:3]=[C:4]2[C:15]([O:17][CH3:18])=[O:16])=[CH:9][CH:10]=1
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참가 물질

8

반응물 4

HCID 6228DimethylformamideHCID 10340Sodium CarbonateHCID 78412Phenyl dihydrogen orthoborateHCID 58306731methyl 4-bromo-1-(4-chlorobenzyl)-1H-pyrrole-2-carboxylate

생성물 1

HCID 58306767methyl 1-(4-chlorobenzyl)-4-phenyl-1H-pyrrole-2-carboxylate수율 36.7%

시약·촉매·용매 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
촉매
HCID 962Water용매2회
HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

To a mixture of methyl 4-bromo-1-(4-chlorobenzyl)-1H-pyrrole-2-carboxylate (0.72 g) and DMF (21 mL) were added phenylboric acid (0.30 g), sodium carbonate (0.58 g), water (3.0 mL), and tetrakis(triphenylphosphine) palladium (0.13 g), followed by stirring at 100° C. for 24 hours. To the reaction mixture were added ethyl acetate and water, and the insoluble materials were separated by filtration through Celite. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=0 to 10%) to obtain methyl 1-(4-chlorobenzyl)-4-phenyl-1H-pyrrole-2-carboxylate (0.26 g).

후처리

  1. customthe insoluble materials were separated by filtration through Celite
  2. washThe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane=0 to 10%)

출처 및 근거

ORD 기록
ord-41c9e67cb03f47c0b0d706c6b2563bd7
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598355B2

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