反応 #1869217

反応方程式

AlCl3

4-tert-butyl-2-methoxybenzenesulfonyl chloride

pyrrolidine

→

subtitle compound

収率 53.3%

2-(pyrrolidin-1-ylsulfonyl)phenol

収率 53.3%

溶媒

xylene

DMF

反応条件

後処理

1. 1
   濃縮concentrated in vacuo
2. 2
   workup.DISSOLUTIONThe residue was dissolved in xylene (10 ml)
3. 3
   workup.STIRRINGThe resulting mixture was stirred for 18 h at 70° C
4. 4
   workup.ADDITIONwas poured
5. 5
   workup.STIRRINGinto stirred ice-cold water
6. 6
   抽出extracted with ether (2×30 ml)
7. 7
   乾燥The ether layer was dried over sodium sulfate
8. 8
   ろ過filtered
9. 9
   濃縮concentrated

実験手順

To a solution of 4-tert-butyl-2-methoxybenzenesulfonyl chloride (258 mg, 0.99 mmol) in DMF (6 ml) was added pyrrolidine (70 mg, 0.99 mmol) and the solution was stirred at ambient temperature for 30 minutes, and concentrated in vacuo. The residue was dissolved in xylene (10 ml) and then added to mixture of AlCl3 (525 mg, 3.39 mmol) in xylene (5 ml). The resulting mixture was stirred for 18 h at 70° C. After colling the mixture was poured into stirred ice-cold water, and extracted with ether (2×30 ml). The ether layer was dried over sodium sulfate, filtered and concentrated to give 120 mg of subtitle compound.

出典