Potassium Carbonate → HCID 86666271、化合物

HRID 1026239ノート

反応式

HRID 1026239 の反応式
Br[CH2:2][CH:3]1[CH2:5][CH2:4]1.[Br:6][C:7]1[CH:12]=[C:11]([OH:13])[CH:10]=[CH:9][C:8]=1[CH2:14][C:15]([OH:17])=[O:16].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Br:6][C:7]1[CH:12]=[C:11]([O:13][CH2:2][CH:3]2[CH2:5][CH2:4]2)[CH:10]=[CH:9][C:8]=1[CH2:14][C:15]([O:17][CH2:2][CH:3]1[CH2:5][CH2:4]1)=[O:16]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 24721648(2-Bromo-4-hydroxyphenyl)acetic acid

生成物 1

HCID 86666271HCID 86666271、化合物収率 89.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of (bromomethyl)cyclopropane (10.52 g), (2-bromo-4-hydroxyphenyl)acetic acid (6.0 g) and potassium carbonate (7.18 g) in DMF (200 mL) was stirred at 80° C. for 8 hr. The reaction mixture was allowed to cool to room temperature, and the solvent was evaporated under reduced pressure. The residue was diluted with diethyl ether and water, and the organic layer was separated. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (7.89 g).

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. additionThe residue was diluted with diethyl ether and water
  3. customthe organic layer was separated
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-94c7ae5292e242dc90446a9558102a27
出典データセット
uspto-grants-2014_05
特許番号
US08729102B2

反応ノート

読み込み中…