반응 #2006426

ord-c618f662dbbb4b3daba72fb92202f9f0

반응 방정식

CI
methyl iodide
O=S(=O)(Nc1ccc(I)cc1)c1ccccc1
compound 28
O=S(=O)(Nc1ccc(I)cc1)c1ccccc1
4-(Benzenesulfonylamino)-phenyl Iodide
O=C([O-])[O-].[K+].[K+]
K2CO3
CNS(=O)(=O)c1ccccc1-c1ccc(I)cc1
title compound
수율 196.6%
CNS(=O)(=O)c1ccccc1-c1ccc(I)cc1
N-Methyl-4-iodophenylbenzenesulfonamide
수율 196.6%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The resulting reaction mixture
  2. 2
    기타The solvent is then removed
  3. 3
    workup.ADDITIONwater was added
  4. 4
    추출The resulting mixture was extracted with ethyl acetate
  5. 5
    기타the combined organic phases were dried
  6. 6
    농축concentrated
  7. 7
    기타Purification by flash chromatography

실험 절차

To compound 28 (from Example 18) (500 mg, 1.39 mmol) in DMF (10 mL) were added at room temperature K2CO3 (962 mg, 6.96 mmol), followed by methyl iodide (395 mg, 2.78 mmol). The resulting reaction mixture was stirred at room temperature for 16 hours. The solvent is then removed and water was added. The resulting mixture was extracted with ethyl acetate, and the combined organic phases were dried and concentrated. Purification by flash chromatography using hexane:ethyl acetate (8:2) afforded 510 mg (98%) of the title compound as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE043343E1uspto-grants-2012_05