반응 #460622

반응 방정식

phthalic acid

2-cyano-2-(1-ethoxycarbonyl-1-methylethoxyimino)acetamidine

potassium thiocyanate

bromine

→

2-(5-amino-1,2,4-thiadiazol-3-yl)-2-(1-ethoxycarbonyl-1-methylethoxyimino)acetonitrile

용매

methanol

water

N,N-dimethylformamide

methanol

triethylamine

반응 조건

후처리

1. 1
   기타at -15°~10° C
2. 2
   workup.STIRRINGthe mixture was stirred for one hour under ice-
3. 3
   온도cooling
4. 4
   여과The resulting precipitate was collected by filtration
5. 5
   세척washed with cold water (60 ml)
6. 6
   기타dried under reduced pressure

실험 절차

To a suspension of phthalic acid salt (10.0 g) of 2-cyano-2-(1-ethoxycarbonyl-1-methylethoxyimino)acetamidine in methanol (60 ml) were added dropwise triethylamine (9.01 g) and bromine (3.67 g) at -15°~10° C. After stirring for 15 minutes at the same temperature, N,N-dimethylformamide (6.0 ml) and a solution of potassium thiocyanate (2.23 g) in methanol (22.3 ml) were added dropwise thereto at -15°~10° C. After stirring for one hour at -5°~0° C., the solution was poured into cold water (300 ml) and the mixture was stirred for one hour under ice-cooling. The resulting precipitate was collected by filtration, washed with cold water (60 ml) and dried under reduced pressure to give 2-(5-amino-1,2,4-thiadiazol-3-yl)-2-(1-ethoxycarbonyl-1-methylethoxyimino)acetonitrile (3.82 g).

출처