反応 #63160

反応方程式

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

収率 85.3%

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

収率 85.3%

溶媒

acetonitrile

water

反応条件

後処理

1. 1
   ろ過The resulting precipitate was collected by filtration
2. 2
   洗浄washed well with water and ether

実験手順

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).

出典