반응 #60211

ord-c48126b04fd44e2e8d3256f52bdec051

반응 조건

온도
23°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the resulting solution was maintained at 23° C. for 5 min.
  2. 2
    여과filtered
  3. 3
    세척washed with NMP, H2O and CH2Cl2 and air
  4. 4
    기타dried

실험 절차

To a solution of Ph3P (11 g, 42 mmol) and CH2Cl2 (20 mL) at 23° C. was added DIAD (6.6 mL, 42 mmol) and the resulting yellow solution was maintained at 23° C. for 30 min. To this solution was added 2-(dimethylamino)-ethanol (4.2 mL, 42 mmol) and the resulting solution was maintained at 23° C. for 5 min. then added to a suspension of resin-bound {2-[(5-nitro(2-pyridyl))amino]ethyl}[(2-nitrophenyl)sulfonyl]amine (3.0 g, 2.1 mmol) and CH2Cl2 (30 mL). The resulting mixture was shaken at 23° C. for 12 h, filtered, washed with NMP, H2O and CH2Cl2 and air dried to yield polymer-bound [2-(dimethylamino)ethyl]{2-[(5-nitro(2-pyridyl))amino]ethyl}[(2-nitrophenyl)sulfonyl]amine.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425557B2uspto-grants-2008_09