Hydrochloric Acid → 2-(Pyridin-3-YL)-[1,2,4]triazolo[1,5-A]pyridin-6-amine

HRID 588421노트

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HRID 588421 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:23]=[C:10]3[CH:11]=[CH:12][C:13]([NH:15]C(=O)OC(C)(C)C)=[CH:14][N:9]3[N:8]=2)[CH:2]=1.Cl.C(OCC)C>ClCCl>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:23]=[C:10]3[CH:11]=[CH:12][C:13]([NH2:15])=[CH:14][N:9]3[N:8]=2)[CH:2]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 89464387Tert-butyl 2-(pyridin-3-yl)-[1,2,4]triazolo[1,5-a]pyridin-6-ylcarbamate

생성물 1

HCID 717437892-(Pyridin-3-YL)-[1,2,4]triazolo[1,5-A]pyridin-6-amine수율 53.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

A mixture of tert-butyl 2-(pyridin-3-yl)-[1,2,4]triazolo[1,5-a]pyridin-6-ylcarbamate (1.34 g, 4.3 mmol), dichloromethane (10 ml) and hydrochloric acid (5 molar in diethyl ether (36.0 g, 30 ml, 987 mmol) was stirred for 18 hours at 25° C. The solvents were evaporated under reduced pressure and the residue treated with sodium hydroxide solution (2 molar in water). The mixture was extracted with ethyl acetate, the organic layers were washed with water and brine, dried over magnesium sulfate, filtrated and evaporated to dryness, affording 2-pyridin-3-yl-[1,2,4]triazolo[1,5-a]pyridin-6-ylamine (482 mg, 53%) as light brown solid. Mp.: 230° C. MS: m/z=212.1 (M+H+).

후처리

  1. customThe solvents were evaporated under reduced pressure
  2. additionthe residue treated with sodium hydroxide solution (2 molar in water)
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe organic layers were washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltrated
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-0972373d06274224a0852bf9aac234f5
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227970B2

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