Water → HCID 59557783、化合物

HRID 2038475ノート

反応式

HRID 2038475 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

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 517045Sodium AcetateHCID 595577434-Bromo-2-(4-(bromomethyl)benzyl)-1-chlorobenzene

生成物 1

HCID 59557783HCID 59557783、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

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-1be56de5acf54da48dc29f2fe6d07a1b
出典データセット
uspto-grants-2013_11
特許番号
US08575321B2

反応ノート

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