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

HRID 465115ノート

反応式

HRID 465115 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-db9af6fd3a9f4d898db18d8f8c613664
出典データセット
uspto-grants-1985_10
特許番号
US04550166

反応ノート

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