反应 #710466

ord-ffdd7d0ce13447fcab851325e1354a4c

反应方程式

Cl.N=c1ccccn1Cc1ccc(Cl)nc1
1-[(6-chloropyridin-3-yl)methyl]pyridin-2(1H)-imine hydrochloride
CCN=C=NCCCN(C)C.Cl
EDC-HCl
O=C(O)C(Br)Br
dibromoacetic acid
O=C(N=c1ccccn1Cc1ccc(Cl)nc1)C(Br)Br
2,2-dibromo-N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-acetamide
收率 15.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed once with water and twice with a 1% HCl aqueous solution
  2. 2
    干燥dried over anhydrous magnesium sulfate
  3. 3
    浓缩concentrated under reduced pressure
  4. 4
    其他to obtain the subject material
  5. 5
    其他Amount obtained 50 mg (yield 15%)

实验过程

200 mg (0.78 mmol) of the 1-[(6-chloropyridin-3-yl)methyl]pyridin-2(1H)-imine hydrochloride obtained by the method described in another method of Synthetic Example P1, 238 mg (1.95 mmol) of DMAP and 224 mg (1.17 mmol) of EDC-HCl were dissolved in 10 ml of anhydrous dichloromethane, 101 μl (202 mg, 1.17 mmol) of dibromoacetic acid was added thereto, and the resulting mixture was stirred at room temperature overnight. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed once with water and twice with a 1% HCl aqueous solution, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain the subject material. Amount obtained 50 mg (yield 15%)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09301525B2uspto-grants-2016_04