Ethyl orthoformate → 8-(3-Pyridinyl)-1,2,4-triazolo[4,3-a]pyridine

HRID 465115노트

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HRID 465115 반응식
[NH:1]([C:3]1[C:8]([C:9]2[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=2)=[CH:7][CH:6]=[CH:5][N:4]=1)[NH2:2].[CH:15](OCC)(OCC)OCC>>[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]([C:8]2[C:3]3[N:4]([CH:15]=[N:2][N:1]=3)[CH:5]=[CH:6][CH:7]=2)[CH:10]=1

참가 물질

3

반응물 2

HCID 31214Ethyl orthoformateHCID 135337152-Hydrazino-3,3'-bipyridine

생성물 1

HCID 135337048-(3-Pyridinyl)-1,2,4-triazolo[4,3-a]pyridine

반응 조건

온도
100 °C

실험 절차

A 4.15 g portion of 2-hydrazino-3,3'-bipyridine was dissolved in 30 ml of triethyl orthoformate and heated at 100° C. for 2 hours. The volatiles were removed at reduced pressure and the residue purified by chromatography on hydrous magnesium silicate, eluting with ethyl acetate. The solid was recrystallized from methylene chloride-hexane, giving 2.67 g of the desired product, mp 186°-189° C.

후처리

  1. customThe volatiles were removed at reduced pressure
  2. customthe residue purified by chromatography on hydrous magnesium silicate
  3. washeluting with ethyl acetate
  4. customThe solid was recrystallized from methylene chloride-hexane

출처 및 근거

ORD 기록
ord-db9af6fd3a9f4d898db18d8f8c613664
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550166

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