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

HRID 1513013
ノート
印刷プレビュー

反応式

HRID 1513013 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 167845
palladium(II) acetate
触媒
HCID 6342Acetonitrile溶媒
HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-ba9727349bfd492a84534f64315817b7
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217069B2

反応ノート

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