تفاعل #2028952

معادلة التفاعل

11

8-amino-9,10-difluoro-3,3-dimethyl-7-oxo-3,7-dihydro-2H-(1,4)oxazino(2,3,4-ij)quinoline-6-carboxamide

triethylamine

POCl3

→

12

المردود 94.6%

8-amino-9,10-difluoro-3,3-dimethyl-7-oxo-3,7-dihydro-2H-(1,4)oxazino(2,3,4-ij)quinoline-6-carbonitrile

المردود 94.6%

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGThe mixture was stirred an additional 5 h at 0° C
2. 2
   أخرىUpon completion of the reaction
3. 3
   أخرىthe solvent was removed by evaporation
4. 4
   workup.ADDITION70 mL of water were added
5. 5
   workup.STIRRINGthe mixture stirred at room temperature for 1 h
6. 6
   أخرىThe precipitate that formed
7. 7
   ترشيحwas collected by filtration
8. 8
   غسيلwashed with water
9. 9
   أخرىThe solid was dried under vacuum

الإجراء التجريبي

A mixture of 11 (2.92 g, 9.44 mmol) and triethylamine (6.6 mL, 47 mmol) in CH2Cl2 (20 ml) was cooled to 0° C. and POCl3 (4.35 g, 28 mmol) was added drop wise with stirring. The mixture was stirred an additional 5 h at 0° C. During that time, the reaction mixture turned dark-brown. Upon completion of the reaction, the solvent was removed by evaporation. 70 mL of water were added and the mixture stirred at room temperature for 1 h. The precipitate that formed was collected by filtration and washed with water. The solid was dried under vacuum to yield 12 as a brown solid (2.6 g, 94%). This compound was used without further purification in the next step.

المصدر