反应 #2843

ord-f4e8e6ec20fc45b7ba597aed2b56cab8

反应方程式

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
收率 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
收率 96.7%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The layers are separated
  2. 2
    洗涤The organic layer is washed with H2O and saturated NaCl
  3. 3
    干燥The organic layer is dried over MgSO4
  4. 4
    过滤filtered
  5. 5
    浓缩concentrated
  6. 6
    其他The residue is triturated with Et2O

实验过程

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.

来源

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