반응 #9444

반응 방정식

7-Bromo-3-nitroquinolin-4-ol

POCl3

→

7-bromo-4-chloro-3-nitroquinoline

반응 조건

후처리

1. 1
   기타brought to 102° C. under an atmosphere of N2
2. 2
   workup.DISSOLUTIONall of the solids had dissolved, so the reaction
3. 3
   여과The resulting solids were collected by filtration
4. 4
   세척washed with H2O
5. 5
   기타partitioned with CH2Cl2 (3 L) and 2M Na2CO3 (500 mL)
6. 6
   기타The organic layer was separated
7. 7
   세척washed with H2O (1×)
8. 8
   건조dried over Na2SO4
9. 9
   여과filtered
10. 10
    농축concentrated

실험 절차

7-Bromo-3-nitroquinolin-4-ol (42 g, 156 millimoles (mmol)) was suspended in POCl3 (130 mL) and brought to 102° C. under an atmosphere of N2. After 45 min, all of the solids had dissolved, so the reaction was cooled to room temperature (RT). The resulting solids were collected by filtration, washed with H2O, and then partitioned with CH2Cl2 (3 L) and 2M Na2CO3 (500 mL). The organic layer was separated, washed with H2O (1×), dried over Na2SO4, filtered, and concentrated to afford 33.7 g of 7-bromo-4-chloro-3-nitroquinoline as a beige solid.

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