Sodium Hydroxide → 2-butyl-5-chloro-1H-imidazole

温度

100 °C

2-n-Butyl-3,5-dihydroimidazol-4-one (14.02 g, 0.1 mol) was added in portions for 15 minutes to POCl3 (50 ml) at 95° C. The solution was heated for 2 hours at 100° C., cooled and poured on 400 g of ice. The mixture was adjusted to pH 7 with 255 ml of 30 percent sodium hydroxide solution and extracted three times with 500 ml of ethyl acetate each. The combined organic phases were dried with MgSO4, filtered and concentrated by evaporation on a Rotavapor. After purification of the residue by column chromatography the title compound (5.52 g, 34.7 percent) was obtained in a high yield (>98 percent, according to GC and 1H-NMR). The product had a melting point of 85° to 87° C. Other data regarding the product was:

1. temperaturecooled
2. extractionextracted three times with 500 ml of ethyl acetate each
3. dry with materialThe combined organic phases were dried with MgSO4
4. filtrationfiltered
5. concentrationconcentrated by evaporation on a Rotavapor
6. customAfter purification of the residue by column chromatography the title compound (5.52 g, 34.7 percent)
7. customwas obtained in
8. customa high yield (>98 percent, according to GC and 1H-NMR)

ORDレコード

ord-b08da4ae275c450389d9685c88538f56

出典データセット

uspto-grants-1996_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05508425