反应 #1869201

ord-2034badeb438445dac16877f59b9ef1e

反应方程式

O=c1[nH]c2ccccc2cc1Cl
chloroquinolone
CN(C)C=O
DMF
BrP(Br)Br
phosphorus tribromide
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
Clc1cnc2ccc3c(c2c1Br)OCCO3
solid
Clc1cnc2ccc3c(c2c1Br)OCCO3
10-Bromo-9-chloro-2,3-dihydro-[1,4]dioxino[2,3-f]quinoline

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooling for 30 minutes
  2. 2
    workup.STIRRINGstirred for a further 2 hours
  3. 3
    温度It was cooled in ice
  4. 4
    其他the solid was collected
  5. 5
    洗涤washed well with water
  6. 6
    其他dried in vacuo

实验过程

The chloroquinolone (7a) in dry DMF (8 mL) was cooled in ice and phosphorus tribromide (0.7 mL) added drop-wise, and the mixture was stirred, with ice-cooling for 30 minutes then allowed to warm to room temperature and stirred for a further 2 hours. It was cooled in ice and sodium carbonate solution was added and the solid was collected, washed well with water, and dried in vacuo, to afford a pale yellow solid (1.65 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07498326B2uspto-grants-2009_03