HRID902721

反应详情

EQUATION

反应方程式

HRID 902721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-Methyl-3-hydroxybenzene sulfonamide (175 mg, 0.94 mmole) in 15 mL of DMF was treated with Cs2CO3 (305 mg, 0.94 mmole), and stirred for 45 minutes. A solution of 3-Chloro-1-propanol tosylate (223 mg, 0.90 mmole) in 3 mL of DMF was added. The reaction was heated at 55° for 3 hours, and stirred at 23° for 16 hours. The reaction was diluted with H2O and extracted with Et2O. The extracts were washed with H2O, dried and the solvent removed. The residue was chromatographed on a silica gel column, and elution with 30% EtOAc in hexane gave the titled product, 75 mg (30%). MS (ESI) 264 (MH+).

WORKUP

后处理

  1. temperatureThe reaction was heated at 55° for 3 hours
  2. stirringstirred at 23° for 16 hours
  3. extractionextracted with Et2O
  4. washThe extracts were washed with H2O
  5. customdried
  6. customthe solvent removed
  7. customThe residue was chromatographed on a silica gel column, and elution with 30% EtOAc in hexane