1,1,1-Triethoxybutane → 4-Chloro-1-propyl[1,2,4]triazolo[4,3-a]quinoxaline

HRID 2412900

반응식

HRID 2412900 반응식
[Cl:1][C:2]1[C:11]([NH:12][NH2:13])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[C:14](OCC)(OCC)(OCC)[CH2:15][CH2:16][CH3:17]>>[Cl:1][C:2]1[C:11]2[N:10]([C:14]([CH2:15][CH2:16][CH3:17])=[N:13][N:12]=2)[C:9]2[C:4]([N:3]=1)=[CH:5][CH:6]=[CH:7][CH:8]=2

참가 물질

3

반응물 2

HCID 3717791,1,1-TriethoxybutaneHCID 36588202-Chloro-3-hydrazinoquinoxaline

생성물 1

HCID 133857074-Chloro-1-propyl[1,2,4]triazolo[4,3-a]quinoxaline수율 53%

실험 절차

2-Chloro-3-hydrazinoquinoxaline (3.0 g., 0.015 mole), the product of Example 1, was stirred with triethyl orthobutyrate (27 ml.) at 100° C. for 2 hours. The mixture was cooled to room temperature, and the precipitate was collected by filtration and washed with cyclohexane. The crude solid was taken up in chloroform and filtered to remove insoluble material. The chloroform solution was concentrated in vacuo to give a solid which was recrystallized from chloroform to give 1.96 g. (53% yield) of 4-chloro-1-n-propyl-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. 173°-175° C. Mass spectrum: m/e, 246 (P).

후처리

  1. filtrationthe precipitate was collected by filtration
  2. washwashed with cyclohexane
  3. filtrationfiltered
  4. customto remove insoluble material
  5. concentrationThe chloroform solution was concentrated in vacuo
  6. customto give a solid which
  7. customwas recrystallized from chloroform
  8. customto give 1.96 g

출처 및 근거

ORD 기록
ord-8a7a15016f7e4ef2b54766f480629944
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04495187

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