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Hydrochloric Acid → Ethyl 5-chloro-2-(2,3-difluoro-6-methoxybenzyloxy)-4-nitrocinnamate

HRID 1513013
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HRID 1513013 반응식
Br[C:2]1[C:7]([O:8][CH2:9][C:10]2[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=2[F:19])=[CH:6][C:5]([N+:20]([O-:22])=[O:21])=[C:4]([Cl:23])[CH:3]=1.[C:24]([O:28][CH2:29][CH3:30])(=[O:27])[CH:25]=[CH2:26].CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.Cl>C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(N(CC)CC)C>[Cl:23][C:4]1[C:5]([N+:20]([O-:22])=[O:21])=[CH:6][C:7]([O:8][CH2:9][C:10]2[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=2[F:19])=[C:2]([CH:3]=1)[CH:26]=[CH:25][C:24]([O:28][CH2:29][CH3:30])=[O:27]
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 8821Ethyl AcrylateHCID 80271Tri-o-tolylphosphineHCID 685153834-Bromo-2-chloro-5-(2,3-difluoro-6-methoxybenzyloxy)-1-nitrobenzene

생성물 1

HCID 68514028Ethyl 5-chloro-2-(2,3-difluoro-6-methoxybenzyloxy)-4-nitrocinnamate

시약·촉매·용매 3

HCID 167845
palladium(II) acetate
촉매
HCID 6342Acetonitrile용매
HCID 8471Triethylamine용매

실험 절차

A mixture of 4-bromo-2-chloro-5-(2,3-difluoro-6-methoxybenzyloxy)-1-nitrobenzene (3.06 g), ethyl acrylate (1.64 mL), palladium(II) acetate (84 mg), tris(2-methylphenyl)phosphine (0.23 g) and triethylamine (5.2 mL) in acetonitrile (30 mL) was heated at reflux overnight. The reaction mixture was cooled to room temperature, and poured into 1 mol/L hydrochloric acid, and the resulting mixture was extracted with ethyl acetate. The extract was washed with water and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=4/1−2/1) to give ethyl 5-chloro-2-(2,3-difluoro-6-methoxybenzyloxy)-4-nitrocinnamate (2.46 g). This material was dissolved in tetrahydrofuran (30 mL). To the solution were added methanol (30 mL) and nickel(II) bromide (63 mg). To the mixture was added sodium borohydride (0.65 g) under ice-cooling, and the mixture was stirred at the same temperature for 30 minutes, and then stirred at room temperature for 30 minutes. The reaction mixture was poured into a saturated aqueous sodium hydrogen carbonate solution, and the resulting mixture was extracted with ethyl acetate. The extract was washed with water and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=4/1−1/1) to give the title compound (0.69 g).

후처리

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. extractionthe resulting mixture was extracted with ethyl acetate
  4. washThe extract was washed with water and brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=4/1−2/1)

출처 및 근거

ORD 기록
ord-ba9727349bfd492a84534f64315817b7
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217069B2

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