반응 #1256702

반응 방정식

5-amino-4-cyano-3-methylisothiazole

sodium nitrite

water

→

4-cyano-3-methyl-5-nitrosoaminoisothiazole

용매

formic acid

반응 조건

후처리

1. 1
   workup.ADDITIONAfter completion of dropwise addition
2. 2
   workup.STIRRINGthe mixture was continuously stirred at 0° C. further for one hour
3. 3
   기타to precipitate crystals, which
4. 4
   여과were collected by filtration
5. 5
   세척washed with ice cold water
6. 6
   기타The crystals were dried in the air at room temperature overnight

실험 절차

First, 4 g (0.028 mol) of 5-amino-4-cyano-3-methylisothiazole was dissolved in 40 mL of 98% formic acid. While the mixture was stirred, an aqueous sodium nitrite solution (containing 2.1 g (0.03 mmol) of sodium nitrite in 6 mL of water) was added dropwise at 0° C. or less. After completion of dropwise addition, the mixture was continuously stirred at 0° C. further for one hour. To the solution, 100 mL of water was added to precipitate crystals, which were collected by filtration and washed with ice cold water. The crystals were dried in the air at room temperature overnight to obtain 2.6 g (56% in yield) of 4-cyano-3-methyl-5-nitrosoaminoisothiazole. To 2 g (0.012 mol) of the obtained nitrosoaminoisothiazole, 20 mL of methanol was added, stirred while heating to an inner temperature of 55 to 60° C. for one hour and cooled to room temperature to precipitate crystals, which were collected by filtration. The crystals were recrystallized from methanol to obtain 0.66 g (41% in yield) of triazene dissociative direct dye D-34.

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