تفاعل #51143

معادلة التفاعل

water

ethanol

sodium borohydride

1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylchloromethylimino)pyrazole-3-carbonitrile

→

1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylmethylamino)pyrazole-3-carbonitrile

المردود 92.4%

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىat 20° C. or less
2. 2
   أخرىto precipitate crystals
3. 3
   workup.STIRRINGAfter 30 minutes of stirring
4. 4
   ترشيحthe crystals were filtrated
5. 5
   غسيلwashed with water until the pH of the filtrate
6. 6
   أخرىThe crystals thus obtained
7. 7
   استخلاصthe solution was extracted
8. 8
   workup.ADDITIONafter the addition of saturated saline
9. 9
   تجفيفThe organic layer was dried over anhydrous magnesium sulfate
10. 10
    ترشيحfiltrated
11. 11
    تركيزconcentrated
12. 12
    ترشيحThe resulting crystals were filtrated
13. 13
    غسيلwashed with a small amount of hexane and ethyl acetate
14. 14
    أخرىdried

الإجراء التجريبي

To an ethanol (2 ml) suspension of 85 mg (2.2 mmol) of sodium borohydride was gradually added 0.5 g (1.1 mmol) of 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylchloromethylimino)pyrazole-3-carbonitrile at 20° C. or less. After 1 hour of stirring at room temperature, the mixture was gradually poured into 40 ml of water to precipitate crystals. After 30 minutes of stirring, the crystals were filtrated and washed with water until the pH of the filtrate became 6. The crystals thus obtained were dissolved in ethyl acetate and the solution was extracted after the addition of saturated saline. The organic layer was dried over anhydrous magnesium sulfate, filtrated, and concentrated. The resulting crystals were filtrated, washed with a small amount of hexane and ethyl acetate, and dried to obtain 0.42 g (yield 92%) of 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylmethylamino)pyrazole-3-carbonitrile.

المصدر