반응 #171914

ord-0d9589c7e058451894f1ce443e0d8999

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The reaction mixture was then washed with 2N NaOH, water, brine
  2. 2
    건조dried over Na2SO4
  3. 3
    기타Solvent was removed in vacuo

실험 절차

EDCI (7.07 g, 36.9 mmol) was added in one portion to a stirred solution of 3-Iodo-5-nitro-benzoic acid (2.31 g, 24.6 mmol), HOBt (4.985 g, 36.9 mmol), 2-Amino-1-methoxypropane (2.73 ml, 24.6 mmol) and NMP (4.06 ml 36.9 mmol) in CH2Cl2 (120 ml) and DMF (10 ml) at 0° C. The reaction was allowed to warm to room temperature and was stirred over night. The reaction mixture was then washed with 2N NaOH, water, brine, and dried over Na2SO4. Solvent was removed in vacuo to give 2.50 g of 3-Iodo-N-(2-methoxy-1-methyl-ethyl)-5-nitro-benzamide as a yellow solid, MS (M+H)=365. This material was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846945B2uspto-grants-2014_09