反应 #5930

反应方程式

chloroacetyl chloride

1-amino-2-naphthol

N,N-dimethylaniline

tetrahydrofuran

→

1H-naphtho[2,1-b][1,4]oxazin-2(3H)-one

溶剂

ethyl acetate

反应条件

后处理

1. 1
   洗涤the ethyl acetate layer is washed
2. 2
   其他dried
3. 3
   workup.DISTILLATIONdistilled
4. 4
   其他to remove the solvent
5. 5
   workup.DISSOLUTIONThe resulting oil is dissolved in acetone (500 ml)
6. 6
   workup.ADDITIONis added potassium carbonate (75 g)
7. 7
   温度the mixture is refluxed for 2 hours
8. 8
   workup.DISTILLATIONacetone is distilled off
9. 9
   workup.ADDITIONTo the residue is added water
10. 10
    其他the precipitate is separated by filtration
11. 11
    洗涤washed
12. 12
    其他dried
13. 13
    其他recrystallized from tetrahyrofuran

实验过程

To a mixture of 1-amino-2-naphthol (16.9 g), N,N-dimethylaniline (19.3 g) and tetrahydrofuran (200 ml) is added dropwise chloroacetyl chloride under ice cooling, and the mixture is stirred at the same temperature for one hour. To the reaction mixture is added ethyl acetate, and the ethyl acetate layer is washed, dried and distilled to remove the solvent. The resulting oil is dissolved in acetone (500 ml) and thereto is added potassium carbonate (75 g), and the mixture is refluxed for 2 hours, and acetone is distilled off. To the residue is added water, and the precipitate is separated by filtration, washed, dried and recrystallized from tetrahyrofuran to give 1H-naphtho[2,1-b][1,4]oxazin-2(3H)-one (13.1 g). M.p. 219°-220.5° C.

来源