반응 #2377511

반응 방정식

Sodium borohydride

3-[4-(2-hydroxyethyl)-1-piperazinyl]-5-methyl-6-phenyl-1,2,4-triazine

→

3-[4-(2-hydroxyethyl)-1-piperazinyl]-5-methyl-6-phenyl-2,5-dihydro-1,2,4-triazine

수율 62.9%

용매

methanol

반응 조건

후처리

1. 1
   여과The reaction mixture was filtered by suction
2. 2
   기타the filtrate was evaporated
3. 3
   추출The resultant residue was extracted with ethyl acetate
4. 4
   workup.ADDITIONafter addition of water
5. 5
   세척the extract was washed with brine
6. 6
   건조dried over sodium sulfate
7. 7
   농축concentrated to a small volume
8. 8
   기타The resultant precipitates
9. 9
   여과were collected by filtration
10. 10
    세척washed with diisopropyl ether
11. 11
    기타recrystallized from a mixture of ethyl acetate and diisopropyl ether

실험 절차

Sodium borohydride (2.72 g) was added portionwise to a stirred solution of 3-[4-(2-hydroxyethyl)-1-piperazinyl]-5-methyl-6-phenyl-1,2,4-triazine (3.6 g) in methanol (15 ml) at room temperature. The reaction mixture was filtered by suction and the filtrate was evaporated. The resultant residue was extracted with ethyl acetate after addition of water, and the extract was washed with brine, dried over sodium sulfate and concentrated to a small volume. The resultant precipitates were collected by filtration, washed with diisopropyl ether and recrystallized from a mixture of ethyl acetate and diisopropyl ether to give 3-[4-(2-hydroxyethyl)-1-piperazinyl]-5-methyl-6-phenyl-2,5-dihydro-1,2,4-triazine (2.28 g), mp 103°~105° C.

출처