反应 #1365726

ord-4812db38ef61436287b769a9dc9938de

反应方程式

CCCN=C=O
n-Propyl isocyanate
C#CCN1C(=O)COc2cc(F)c(N)cc21
7-fluoro-6-amino-4-(2-propynyl)-2H-1,4-benzoxazin-3(4H)-one
CCCN=C=O
n-propyl isocyanate
C#CCN1C(=O)COc2cc(F)c(NC(=O)NCCC)cc21
N-n-propyl-N′-[7-fluoro-4-(2-propynyl)-2H-1,4-benzoxazin-3(4H)-one-6-yl]urea

溶剂

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the reaction mixture was maintained at 80° C. overnight
  2. 2
    浓缩Then the solution was concentrated to dryness

实验过程

n-Propyl isocyanate (1.0 g, 11.7 mmol) was added to a solution of 7-fluoro-6-amino-4-(2-propynyl)-2H-1,4-benzoxazin-3(4H)-one (0.20 g, 0.9 mmol) in dioxane (20 mL) with stirring. The reaction mixture was heated to 80° C. for 4 hours. More n-propyl isocyanate (0.43 g, 5 mmol) was added and the reaction mixture was maintained at 80° C. overnight. Then the solution was concentrated to dryness to afford N-n-propyl-N′-[7-fluoro-4-(2-propynyl)-2H-1,4-benzoxazin-3(4H)-one-6-yl]urea as a crude intermediate (1.1 g). This was used for the next step without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06444615B1uspto-grants-2002_09