반응 #68682

ord-c075f70a111f43b0b457dcd343c71a4b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas gradually added at −78□, and the reaction mixture
  2. 2
    workup.STIRRINGthe reaction mixture was stirred at room temperature for 17 hours
  3. 3
    기타After the reaction was terminated
  4. 4
    세척the reaction solution was washed with distilled water
  5. 5
    추출extracted with ethyl acetate
  6. 6
    기타purified by column chromatography

실험 절차

Bromobenzene (8.5 g, 0.054 mol) was placed in a flask, and THF (200 ml) was added thereto. After dissolution, n-BuLi (38.4 ml, 0.06 mol) was gradually added at −78□, and the reaction mixture was stirred for one hour at a maintained temperature. Then, 2-bromo-13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione (10 g, 0.024 mol) was added and the reaction mixture was stirred at room temperature for 17 hours. After the reaction was terminated, the reaction solution was washed with distilled water, extracted with ethyl acetate, and purified by column chromatography to give 2-bromo-13,13-dimethyl-6,11-diphenyl-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diol (11 g, yield=82%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08525158B2uspto-grants-2013_09