반응 #169435

ord-2c94fdeb27714705b957ca8d9de3bb7e

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter addition
  2. 2
    여과The solid was filtered
  3. 3
    세척washed with water (250 mL), MeOH (280 mL) and CH2Cl2 (280 mL) sequentially
  4. 4
    기타The solid was dried under vacuum

실험 절차

To a suspension of 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (70.5 g, 0.45 mol) in DCM (1.8 L) was added N-iodosuccinimide (120 g, 0.54 mol) in portions. After addition, the mixture was stirred at room temperature overnight. The solid was filtered and washed with water (250 mL), MeOH (280 mL) and CH2Cl2 (280 mL) sequentially. The solid was dried under vacuum to afford 4-chloro-5-iodo-7H-pyrrolo[2,3-d]pyrimidine as a brown solid in 79% yield, 107 g.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846698B2uspto-grants-2014_09