苯磺酰氯 → 1-(苯基磺酰基)吡咯

HRID 11236

反应方程式

HRID 11236 反应方程式
[H-].[Na+].[NH:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[C:8]1([S:14](Cl)(=[O:16])=[O:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>CN(C=O)C>[C:8]1([S:14]([N:3]2[CH:7]=[CH:6][CH:5]=[CH:4]2)(=[O:16])=[O:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参与物

5

反应物 3

HCID 7369苯磺酰氯HCID 8027吡咯HCID 24758氢化钠

产物 1

HCID 1401461-(苯基磺酰基)吡咯收率 736.9%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂3 次

实验过程

To a suspension of sodium hydride (60% in mineral oil, 2.4 g, 60 mmol) in DMF (100 ml) was added dropwise at an ice bath temperature a solution of pyrrole (3.35 g, 50 mmol) in DMF (5 ml). The mixture was stirred for 30 minutes at room temperature and cooled again. To the mixture was added dropwise a soluton of benzenesulfonylchloride (9.7 g, 5.5 mmol) in DMF (3 ml). The mixture was stirred for 30 minutes at room temperature and poured into ice-water, and extracted with ethylacetate. The extract was washed with water and dried. The solvent was evaporated. The obtained crystal was washed with hexane to give 1-benzenesulfonylpyrrole (8.4 g). Yield: 81%.

后处理

  1. temperaturecooled again
  2. stirringThe mixture was stirred for 30 minutes at room temperature
  3. extractionextracted with ethylacetate
  4. washThe extract was washed with water
  5. customdried
  6. customThe solvent was evaporated
  7. washThe obtained crystal was washed with hexane

来源与证据

ORD记录
ord-a974fa5d025a477aaee1506f61791129
来源数据集
uspto-grants-2006_08
专利号
US07098201B2

关联笔记

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