반응 #1094558

ord-c3f6e35ec8d04909a8eb479871bcf3f7

반응 방정식

O=C1Cc2ccc(Br)cc2N1
6-bromo-2-indolinone
OB(O)Oc1ccccc1
phenylboric acid
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
O=C1Cc2ccc(-c3ccccc3)cc2N1
6-phenyl-2-indolinone

반응 조건

온도
85°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONare added dropwise at ambient temperature
  2. 2
    온도After cooling the catalyst
  3. 3
    여과is filtered off
  4. 4
    세척the residue is washed with 100 ml of water and 20 ml of 1N sodium hydroxide solution
  5. 5
    기타The residue is purified through a silica gel column with petroleum ether/ethyl acetate (8:2) as eluant

실험 절차

2.4 g of 6-bromo-2-indolinone are placed in 60 ml of dimethoxyethane, 1.9 g of phenylboric acid in 8 ml of ethanol and 0.3 g of tetrakistriphenylphosphine palladium are added and to this mixture 12 ml of 2N sodium carbonate solution are added dropwise at ambient temperature. The mixture is stirred for 6 hours at 85° C. After cooling the catalyst is filtered off, the solvent is eliminated and the residue is washed with 100 ml of water and 20 ml of 1N sodium hydroxide solution. The residue is purified through a silica gel column with petroleum ether/ethyl acetate (8:2) as eluant.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06794395B1uspto-grants-2004_09