반응 #8988

ord-94af66816df94b35977fe10338796646

반응 방정식

CCOC(=O)/C(NC(C)=O)=C(\C)N(C)C
(Z)-2-Acetylamino-3-dimethylamino-but-2-enoic acid ethyl ester
NC1CC1
cyclopropylamine
CCOC(=O)/C(NC(C)=O)=C(\C)NC1CC1
(Z)-2-Acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타evaporated under vacuum at 35° C
  2. 2
    workup.ADDITIONWater (30 ml) was added to the residue
  3. 3
    기타evaporated again at 35° C
  4. 4
    기타to obtain the desired crude product as a dark brown oil [MS: m/e=227.4 (M+H+)], which
  5. 5
    기타could be used without any further purification for the next step

실험 절차

(Z)-2-Acetylamino-3-dimethylamino-but-2-enoic acid ethyl ester (4.3 g, 20 mmol) and cyclopropylamine (1.14 g, 20 mmol) were stirred at room temperature in acetic acid (40 ml) for 2 hrs. The reaction mixture was diluted slowly with 30 ml of water and evaporated under vacuum at 35° C. Water (30 ml) was added to the residue and evaporated again at 35° C. The same procedure was repeated twice with toluene (30 ml each) to obtain the desired crude product as a dark brown oil [MS: m/e=227.4 (M+H+)], which could be used without any further purification for the next step.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091222B2uspto-grants-2006_08