반응 #1262

반응 방정식

4-chloro-2,6-diaminopyrimidine

sodium acetate

4-chlorobenzenediazonium chloride

→

6-chloro-5-[(4-chlorophenyl)azo]-2,4-pyrimidinediamine

수율 41.4%

용매

water

acetic acid

반응 조건

후처리

1. 1
   온도with cooling over 30 minutes at a rate that
2. 2
   기타the reaction at 18°
3. 3
   workup.STIRRINGThe reaction was stirred overnight at room temperature
4. 4
   여과the orange crystals were filtered
5. 5
   세척washed with water (4×400 ml)
6. 6
   기타dried in vacuo

실험 절차

To a suspension of 4-chloro-2,6-diaminopyrimidine (21.68 g, 0.150 mol) in water (750 ml) and acetic acid (750 ml) was added sodium acetate (300 g). Solution occurred after stirring for 20 minutes, and then the solution of 4-chlorobenzenediazonium chloride (0.166 mol) was added with cooling over 30 minutes at a rate that kept the reaction at 18°. The reaction was stirred overnight at room temperature, and the orange crystals were filtered, washed with water (4×400 ml), and dried in vacuo to give 17.6 g of 6-chloro-5-[(4-chlorophenyl)azo]-2,4-pyrimidinediamine. The mother liquors were cooled to 5° for 20 hours, and the crystals were collected and dried in vacuo to give 6.94 g of additional 6-chloro-5-[(4-chlorophenyl)azo]-2,4-pyrimidineadiamine.

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