三氟乙酸 → 2-Bromo-1-methyl-1H-pyrrole-3-sulfonamide

HRID 2259183

反应方程式

HRID 2259183 反应方程式
[Br:1][C:2]1[N:3]([CH3:15])[CH:4]=[CH:5][C:6]=1[S:7]([NH:10]C(C)(C)C)(=[O:9])=[O:8].C(O)(C(F)(F)F)=O>C(Cl)Cl>[Br:1][C:2]1[N:3]([CH3:15])[CH:4]=[CH:5][C:6]=1[S:7]([NH2:10])(=[O:8])=[O:9]

参与物

4

反应物 2

HCID 6422三氟乙酸HCID 196938302-bromo-N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide

产物 1

HCID 196938442-Bromo-1-methyl-1H-pyrrole-3-sulfonamide收率 21.4%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

To a solution of 7.11 g (24 mmol) of 2-bromo-N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 50 mL methylene chloride under a nitrogen atmosphere was added 50 mL of TFA. The reaction mixture was allowed to stir at room temperature overnight ca. 16 hours. The reaction mixture was concentrated in vacuo. Three portions of diethyl ether were added to the crude residue and was removed by evaporation to remove residual TFA, which yielded 1.23 g of the title compound as a light brown solid. 1H NMR (Acetone-d6, 200 MHz.) δ: 7.36(d,1H), 6.49(d,1H), 6.3(bs,2H) 3.68(s,3H).

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionThree portions of diethyl ether were added to the crude residue
  3. customwas removed by evaporation
  4. customto remove residual TFA, which

来源与证据

ORD记录
ord-24fca5966e304194948bc21b192c7f7a
来源数据集
uspto-grants-1995_12
专利号
US05472933

关联笔记

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