反応 #1005981

ord-d44c1f39983442608be31b7a06f372af

反応方程式

CS(=O)(=O)CC=CCS(C)(=O)=O
1,4-dimethylsulphonyl-2-butene
COc1ccc(CN)cc1
4-methoxybenzylamine
COc1ccc(CN2CC=CC2)cc1
product
収率 63.6%
COc1ccc(CN2CC=CC2)cc1
1-(4-methoxybenzyl)-3-pyrroline
収率 63.6%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The solid was filtrated
  2. 2
    洗浄the filtrate was washed with water (2×30 ml)
  3. 3
    乾燥dried over Na2SO4
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated
  6. 6
    その他The crude was purified by flash chromatography

実験手順

To a solution of 1,4-dimethylsulphonyl-2-butene (2.15 g, 11.64 mmol) in dichloromethane (40 ml), 4-methoxybenzylamine (6 ml, 44.24 mmol) was added dropwise and the solution was stirred 20 hours at r.t. The solid was filtrated and the filtrate was washed with water (2×30 ml), dried over Na2SO4, filtered and concentrated. The crude was purified by flash chromatography: silica gel, gradient hexane:ethyl acetate 3:1 to 1:1. to afforded the product (1.4 g, 63%) as yellow oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09271959B2uspto-grants-2016_03