反应 #913

ord-ee7d05a9975a483f9332d56b8ce092a7

反应方程式

CSc1c(S(=O)(=O)NC(C)(C)C)ccn1C
N-(1,1-dimethylethyl)-1-methyl-2-(methylthio)-1H-pyrrole-3-sulfonamide
O=C(O)C(F)(F)F
trifluoroacetic acid
CSc1c(S(N)(=O)=O)ccn1C
title compound
收率 79.6%
CSc1c(S(N)(=O)=O)ccn1C
1-Methyl-2-(methylthio)-1H-pyrrole-3-sulfonamide
收率 79.6%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The reaction mixture was concentrated to a tan solid
  2. 2
    workup.ADDITIONDiethyl ether was added to the tan solid
  3. 3
    其他was removed by evaporation
  4. 4
    其他to remove residual TFA
  5. 5
    过滤filtered

实验过程

To a solution of 4.63 g (17.66 mmol) N-(1,1-dimethylethyl)-1-methyl-2-(methylthio)-1H-pyrrole-3-sulfonamide in 50 mL of methylene chloride was added 50 mL of trifluoroacetic acid (TFA) under a nitrogen atmosphere. The orange reaction mixture was stirred at room temperature overnight ca. 16 hours. The reaction mixture was concentrated to a tan solid. Diethyl ether was added to the tan solid and was removed by evaporation to remove residual TFA. The solid was suspended in diethyl ether and filtered giving 2.9 g of the title compound as a solid, m.p. 135°-137° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723410uspto-grants-1998_03