반응 #63160

반응 방정식

hydrochloric acid

product

3-Chloro-2-[(2-oxotetrahydro-3-furanylidene)methyl]-benzenesulfonamide

(4,6-dimethoxy-2-pyrimidinyl)carbamic acid, phenyl ester

1,8-diazabicyclo[5.4.0]undec-7-ene

→

title compound

수율 85.3%

3-Chloro-N-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl]-2-[(2-oxotetrahydro-3-furanylidene)methyl]-benzenesulfonamide

수율 85.3%

용매

acetonitrile

water

반응 조건

후처리

1. 1
   여과The resulting precipitate was collected by filtration
2. 2
   세척washed well with water and ether

실험 절차

To a stirred suspension of 0.15 g (0.0005 mol) of the product of Example 7 and 0.21 g (0.0008 mol) of (4,6-dimethoxy-2-pyrimidinyl)carbamic acid, phenyl ester in 1 mL dry acetonitrile under nitrogen was added dropwise 0.12 mL (0.12 g, 0.0008 mol) of 1,8-diazabicyclo[5.4.0]undec-7-ene. The mixture was stirred at room temperature for 1 hour and was then diluted with water and acidified with 1N aqueous hydrochloric acid. The resulting precipitate was collected by filtration and washed well with water and ether to yield 0.2 g (83%) of the title compound: m.p. 212°-216° (dec); IR (nujol) 3410, 1765, 1605, 1365, 1340, 1155 cm-1 ; NMR (CDCl3, 200 MHz) δ 2.7-2.8 (2H, m), 3.94 (6H, s), 4.1-4.2 (2H, m), 5.84 (1H, s), 7.2-7.8 (3H, m), 8.25 (1H, m).

출처