Water → HCID 59557783、化合物

HRID 1175228ノート

反応式

HRID 1175228 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16]Br)=[CH:12][CH:11]=2)[CH:3]=1.[CH3:18][C:19]([O-:21])=[O:20].[Na+].O.C(OCC)(=O)C>CN(C=O)C>[C:19]([O:21][CH2:16][C:13]1[CH:14]=[CH:15][C:10]([CH2:9][C:4]2[CH:3]=[C:2]([Br:1])[CH:7]=[CH:6][C:5]=2[Cl:8])=[CH:11][CH:12]=1)(=[O:20])[CH3:18]

参加物

6

反応条件

温度
70 °C

実験手順

To a solution of 4-bromo-2-(4-(bromomethyl)benzyl)-1-chlorobenzene (intermediate AI) (15.5 g) in DMF (70 mL), NaOAc (16.27 g) was added. The solution was heated to 70° C. After 3 h, H2O (100 mL) and ethyl acetate (200 mL) were added. The organic layer was separated, washed with brine, and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the product was purified by column chromatography to obtain pure intermediate AJ (8.86 g).

後処理

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried over Na2SO4
  4. customThe solvent was evaporated under reduced pressure
  5. customthe product was purified by column chromatography
  6. customto obtain pure intermediate AJ (8.86 g)

出典と根拠

ORDレコード
ord-68bd2ba77fd240b3a5111cb78e4cdbf8
出典データセット
uspto-grants-2010_11
特許番号
US07838499B2

反応ノート

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