反応 #2843

ord-f4e8e6ec20fc45b7ba597aed2b56cab8

反応方程式

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
収率 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
収率 96.7%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The layers are separated
  2. 2
    洗浄The organic layer is washed with H2O and saturated NaCl
  3. 3
    乾燥The organic layer is dried over MgSO4
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated
  6. 6
    その他The residue is triturated with Et2O

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05731315uspto-grants-1998_03