반응 #1060759

반응 방정식

2,4-dichloro-6-methoxyquinazoline

N-methylaniline

sodium acetate

→

title compound

수율 62.4%

2-Chloro-4-(N-methylphenylamino)-6-methoxyquinazoline

수율 62.4%

용매

tetrahydrofuran

water

반응 조건

후처리

1. 1
   기타Reaction
2. 2
   농축was then concentrated to low volume (about 500 ml)
3. 3
   기타an oil separated out which
4. 4
   여과The solid was filtered off
5. 5
   추출extracted with dichloromethane
6. 6
   기타Silica gel column chromatography followed by evaporation to dryness
7. 7
   기타gave a residue which
8. 8
   세척was washed with 40-60° petroleum ether (to remove trace impurity)

실험 절차

A mixture of 2,4-dichloro-6-methoxyquinazoline, (38.3 g, 0.19M assuming 100% yield from previous step), N-methylaniline (19.26 g, 0.18M), sodium acetate (16.4 g, 0.2M) in tetrahydrofuran (2 liters) and water (1 liter) was stirred at room temperature for 8 days. Reaction was then concentrated to low volume (about 500 ml) and an oil separated out which solidified. The solid was filtered off and extracted with dichloromethane. Silica gel column chromatography followed by evaporation to dryness gave a residue which was washed with 40-60° petroleum ether (to remove trace impurity) to yield title compound (31.25 g) m.p. 133°-134°.

출처