반응 #725908

ord-1e179580f93f4bfaad3d7c1bc13ceb43

반응 방정식

COC(=O)CCCCCOc1ccc(N=C=O)cc1
6-(4-Isocyanato-phenoxy)-hexanoic acid methyl ester
OCCO
ethylene glycol
COC(=O)CCCCCOc1ccc(NC(=O)OCCO)cc1
37
수율 84.0%
COC(=O)CCCCCOc1ccc(NC(=O)OCCO)cc1
6-[4-(2-Hydroxy-ethoxycarbonylamino)-phenoxy]-hexanoic acid methyl ester
수율 84.0%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타rose to 46° C
  2. 2
    여과crude 37 was filtered
  3. 3
    기타dried
  4. 4
    기타recrystallised from toluene

실험 절차

6-(4-Isocyanato-phenoxy)-hexanoic acid methyl ester 36 (15 g, 57 mmol) was added to ethylene glycol (50 ml) at room temperature. The reaction was exothermic and the temperature rose to 46° C. The reaction mixture was allowed to cool to room temperature and later stirred at room temperature for 16 hours. Water (150 ml) was added and crude 37 was filtered, dried and recrystallised from toluene to get pure 37 (12 g, 84%) as a white powder. M.p: 69.5-71.5° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07691364B2uspto-grants-2010_04