反应 #4019

ord-3b3a232422e4466d95c7b4b7201b4772

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to obtain a solution
  2. 2
    其他decanted
  3. 3
    其他to remove a black byproduct residue
  4. 4
    workup.ADDITIONThe filtrate was diluted with water (50 ml)
  5. 5
    其他the resulting yellow precipitate was collected (1.5 g)
  6. 6
    其他A small sample was crystallized from isopropanol (m.p. 115°-118° C.)

实验过程

The commercially available 2-amino-3-hydroxypyridine (5.0 g) and diglyme (30 ml) were heated at 125° C. to obtain a solution. To this solution was added 2-chloro-1,1,1-triethoxyethane (9.9 g) and the mixture was held at 125° for 1 hour. The solution was cooled to room temperature and then decanted to remove a black byproduct residue. The filtrate was diluted with water (50 ml) and the resulting yellow precipitate was collected (1.5 g). A small sample was crystallized from isopropanol (m.p. 115°-118° C.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04723010uspto-grants-1988_02