Reacción #409084

ord-7011ec05a02c49fd83b1c2f270dacd92

Condiciones de reacción

Temperatura
20°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroso obtained from Synthesis example 3
  2. 2
    OtroAfter reaction for 1 hour
  3. 3
    Otroto obtain a white solid
  4. 4
    OtroThe solid, so formed
  5. 5
    Filtraciónwas filtered off
  6. 6
    Lavadowashed with distilled water for dehydration
  7. 7
    workup.DISSOLUTIONdissolved again in acetone
  8. 8
    workup.ADDITIONThen, the reacting solution dropwise added into 5 L water for filtration
  9. 9
    Lavadowashed, for dehydration
  10. 10
    Otrodrying
  11. 11
    OtroThus, a resin, so obtained

Procedimiento

50g of poly(hydroxystyrene/t-butoxycarbonylmethoxystyrene/morpholinylcarbonylmethoxystyrene) where 8.4% of hydroxy groups in polyhydroxystyrene was substituted into t-butoxycarbonylmethoxy group and 5% of hydroxy groups into morpholinylcarbonylmethoxy group, so obtained from Synthesis example 3, was dissolved in 500 ml dimethyl formamide. With the addition of p-toluene sulfonic acid in catalytic amount, the reacting mixture was stirred at 20° C., followed by the addition of ethylvinyl ether (14 g). After reaction for 1 hour, the mixture was neutralized with pyridine, followed by dropwise adding into 5 L water to obtain a white solid. The solid, so formed, was filtered off, washed with distilled water for dehydration and dissolved again in acetone. Then, the reacting solution dropwise added into 5 L water for filtration and washed, for dehydration and drying. Thus, a resin, so obtained, was 52g of poly(hydroxystyrene/ethoxyethoxystyrene/t-butoxycarbonylmethoxystyrene/morpholinocarbonyl lmethoxystyrene) having the weight average molecular weight of 14,400 as polystyrene, in which 16% of hydroxy groups in polyhydroxystyrene was substituted into ethoxyethoxy group, 8.4% of hydroxy groups into t-butoxycarbonylmethoxy group and 5% of hydroxy groups into morpholinylcarbonylmethoxy group.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06210859B1uspto-grants-2001_04