反应 #417901

ord-523b9c4e97b643f8ad5dbfb9b5aeeea5

反应方程式

O=P(Cl)(Cl)Cl
phosphoryl chloride
[O-][n+]1ccnc2c3ccccc3c3ccccc3c21
dibenzo[f,h]quinoxaline-1-oxide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Clc1cnc2c3ccccc3c3ccccc3c2n1
2-Chloro-Dibenzo[f,h]Quinoxaline
收率 93.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他obtained in the above Step 1
  2. 2
    温度while being heated
  3. 3
    温度under reflux for 1 hour
  4. 4
    过滤This solution was filtered
  5. 5
    洗涤the obtained residue was washed with water
  6. 6
    其他methanol to give
  7. 7
    其他the object of the synthesis (as a pale yellow powder in a yield of 93%)
  8. 8
    其他The synthesis scheme of Step 2

实验过程

Next, 18 mL of phosphoryl chloride was dripped into 2.91 g of dibenzo[f,h]quinoxaline-1-oxide obtained in the above Step 1. This mixed solution was stirred while being heated under reflux for 1 hour. This mixed solution was poured into iced water, followed by addition of potassium carbonate so that the mixture was alkaline. This solution was filtered, and the obtained residue was washed with water and then methanol to give the object of the synthesis (as a pale yellow powder in a yield of 93%). The synthesis scheme of Step 2 is illustrated in the following (a″′-2-2).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08877351B2uspto-grants-2014_11