反应 #2125971
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08697604B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 6.55 g (50 mMol) 3-dimethylamino-butyric acid 20 was added to 5.75 g (50 mMol) N-hydroxysuccinimide and 11.05 g (55 mMol) dicyclohexyl carbodiimide in 100 ml CH2Cl2. The reaction mixture was stirred for 16 h at RT. The obtained urea was filtrated and the solution was evaporated. The residue, dissolved in 10 ml acetonitrile, was added under stirring to a solution of 9.51 g (50 mMol) 4-toluenesulfonic acid monohydrate in acetonitrile (30 ml). The solvent was evaporated under vacuum and the product was recrystallized from acetonitrile or acetone. The obtained urea was filtrated the solution was evaporated The residue, dissolved in 10 ml acetonitrile was added The solvent was evaporated under vacuum the product was recrystallized from acetonitrile or acetone
来源 ID: ord-c7059a9b925344ac8b10595ff68b7bbf