반응 #2487410

ord-9c12b277724249c9bb672d83b6bca669

반응 방정식

O=C(O)CCCC[C@@H]1CCSS1
lipoic acid
O=C1CCC(=O)N1O
N-hydroxysuccinimide
ClCCCl
EDC
NC(=O)CCCC[C@@H]1CCSS1
(R)-Lipoamide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with H2O (500 mL), saturated aqueous NaHCO3 (500 mL), saturated aqueous NaCl (500 mL)
  2. 2
    건조dried (MgSO4)
  3. 3
    기타The drying agent was removed by filtration
  4. 4
    농축the filtrate was concentrated to dryness
  5. 5
    기타giving the product as

실험 절차

A solution of lipoic acid (25.6 g, 124 mmol), N-hydroxysuccinimide (15.6 g, 136 mmol), and EDC (26.1 g, 136 mmol) in anhydrous CH2Cl2 (300 mL) was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate (500 mL) and washed with H2O (500 mL), saturated aqueous NaHCO3 (500 mL), saturated aqueous NaCl (500 mL) and dried (MgSO4). The drying agent was removed by filtration and the filtrate was concentrated to dryness giving the product as a yellow sold (35.4 g, 94%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08795706B2uspto-grants-2014_08