반응 #2843

ord-f4e8e6ec20fc45b7ba597aed2b56cab8

반응 방정식

O=C([O-])[O-].[K+].[K+]
K2CO3
N#Cc1cccc(CN2CC[C@H](NS(=O)(=O)c3cc4ccccc4s3)C2=O)c1
benzo[b]thiophene-2-sulfonic acid [1-(3-cyano-benzyl)-2-oxo-pyrrolidin-3-(S)-yl]-amide
CI
methyl iodide
CN([C@H]1CCN(Cc2cccc(C#N)c2)C1=O)S(=O)(=O)c1cc2ccccc2s1
title compound
수율 96.7%
CN([C@H]1CCN(Cc2cccc(C#N)c2)C1=O)S(=O)(=O)c1cc2ccccc2s1
Benzo[b]thiophene-2-sulfonic acid [1-(3-cyanobenzyl)-2-oxo-pyrrolidin-3-(S)-yl]-methylamide
수율 96.7%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The layers are separated
  2. 2
    세척The organic layer is washed with H2O and saturated NaCl
  3. 3
    건조The organic layer is dried over MgSO4
  4. 4
    여과filtered
  5. 5
    농축concentrated
  6. 6
    기타The residue is triturated with Et2O

실험 절차

To a solution of benzo[b]thiophene-2-sulfonic acid [1-(3-cyano-benzyl)-2-oxo-pyrrolidin-3-(S)-yl]-amide (0.25 g, 0.61 mmol) in 3 mL of DMF is added methyl iodide (0.13 g, 0.91 mmol) followed by K2CO3 (0.13 g, 0.91 mmol). The solution is stirred at ambient temperatures for 6 h. After this time, the solution is diluted with H2O and EtOAc. The layers are separated. The organic layer is washed with H2O and saturated NaCl. The organic layer is dried over MgSO4, filtered and concentrated. The residue is triturated with Et2O to give the title compound (0.25 g, 0.59 mmol) as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05731315uspto-grants-1998_03