1,3-Dibromopropane → HCID 86686569、化合物

HRID 1528089ノート

反応式

HRID 1528089 の反応式
[H-].[Na+].[F:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]=1[CH2:13][C:14]([O:16][CH3:17])=[O:15].Br[CH2:19][CH2:20][CH2:21]Br.[Cl-].[NH4+]>CN(C=O)C>[F:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]=1[C:13]1([C:14]([O:16][CH3:17])=[O:15])[CH2:21][CH2:20][CH2:19]1

参加物

6

反応物 4

HCID 80011,3-DibromopropaneHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 86686570HCID 86686570、化合物

生成物 1

HCID 86686569HCID 86686569、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of sodium hydride (9.49 g) in DMF (75 mL) was added dropwise a solution of methyl (2-fluoro-6-nitrophenyl)acetate (23 g) and 1,3-dibromopropane (13.1 mL) in DMF (15 mL) at 0° C. The reaction mixture was stirred at room temperature for 4 hr, cooled to 0° C. Saturated aqueous ammonium chloride solution was added thereto, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (11.3 g).

後処理

  1. temperaturecooled to 0° C
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-823b249abc8e43acad509323b50b7815
出典データセット
uspto-grants-2015_07
特許番号
US09090586B2

反応ノート

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