三氟乙酸 → Methyl 3-(aminosulfonyl)-1-methyl-1H-pyrrole-2-carboxylate

HRID 1081236

反应方程式

HRID 1081236 反应方程式
CC([NH:5][S:6]([C:9]1[CH:13]=[CH:12][N:11]([CH3:14])[C:10]=1[C:15]([O:17][CH3:18])=[O:16])(=[O:8])=[O:7])(C)C.FC(F)(F)C(O)=O>C(Cl)Cl.[Au]>[NH2:5][S:6]([C:9]1[CH:13]=[CH:12][N:11]([CH3:14])[C:10]=1[C:15]([O:17][CH3:18])=[O:16])(=[O:8])=[O:7]

参与物

5

反应物 2

HCID 6422三氟乙酸HCID 19693837Methyl 3-[[(1,1-dimethylethyl)amino]sulfonyl]-1-methyl-1H-pyrrole-2-carboxylate

产物 1

HCID 15790324Methyl 3-(aminosulfonyl)-1-methyl-1H-pyrrole-2-carboxylate

试剂、催化剂与溶剂 2

HCID 23985Gold催化剂HCID 6344二氯甲烷溶剂

实验过程

To a solution of 3.53 g of methyl 3-[[(1,1-dimethylethyl)amino]sulfonyl]-1-methyl-1H-pyrrole-2-carboxylate in 40 mL of methylene chloride under an nitrogen atmosphere was added 80 ml, of trifluoroacetic acid (TFA). The gold solution was stirred at room temperature overnight ca. 16 hours. The gold solution was concentrated to an oily residue. Diethyl ether was added to the residue and removed by evaporation to remove residual TFA. The resulting solid was suspended in diethyl ether and filtered affording the title compound as a tan solid, m.p. 105°-107° C.

后处理

  1. concentrationThe gold solution was concentrated to an oily residue
  2. additionDiethyl ether was added to the residue
  3. customremoved by evaporation
  4. customto remove residual TFA
  5. filtrationfiltered

来源与证据

ORD记录
ord-f2fdda7ab4c84b9aab88acc15e48ddac
来源数据集
uspto-grants-1996_12
专利号
US05585328

关联笔记

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