반응 #1536767

반응 방정식

methanol

choline hydroxide

7-chloro-2,3-dihydro-10-hydroxypyridazino[4,5-b]quinoline-1,4-dione

Toluene

→

title compound

수율 55.0%

7-Chloro-2,3-dihydro-10-hydroxypyridazino[4,5-b]quinoline-1,4-dione Choline Salt

수율 55.0%

용매

water

반응 조건

후처리

1. 1
   농축the mixture was concentrated
2. 2
   기타a rotary evaporator
3. 3
   workup.ADDITIONThe residue was diluted with toluene (250 mL)
4. 4
   농축the resulting mixture concentrated again
5. 5
   기타to provide a yellow residue
6. 6
   여과the resulting suspension was filtered
7. 7
   기타to separate the solids which
8. 8
   세척were washed with methanol (3 mL)
9. 9
   기타dried under a stream of nitrogen for 1 hr
10. 10
    기타Further drying of the solids in vacuo at 100° C. for 20 hr

실험 절차

To a stirred suspension of 7-chloro-2,3-dihydro-10-hydroxypyridazino[4,5-b]quinoline-1,4-dione (1.00 g, 3.8 mM) in water (40 mL) was added choline hydroxide (0.86 mL, 3.8 mM, 50 weight per cent, aqueous solution). Toluene (250 mL) was added to the resulting solution and the mixture was concentrated using a rotary evaporator. The residue was diluted with toluene (250 mL) and the resulting mixture concentrated again to provide a yellow residue. This residue was stirred for 60 hr with methanol (25 mL) and the resulting suspension was filtered to separate the solids which were washed with methanol (3 mL) and then dried under a stream of nitrogen for 1 hr. Further drying of the solids in vacuo at 100° C. for 20 hr provided (0.76 g, 55%) of the title compound as a yellow powder, mp 267°-269° C.

출처