Tetrahydrofuran → 2-Hydrazinylpyridine-4-carbonitrile

HRID 514325

반응식

HRID 514325 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1.O.[NH2:11][NH2:12].C1COCC1>C(O)CCC>[NH:11]([C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1)[NH2:12]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 24654Hydrazine hydrate (1:1)HCID 5686382-Chloro-4-cyanopyridine

생성물 1

HCID 201187142-Hydrazinylpyridine-4-carbonitrile수율 18%

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
60 °C

실험 절차

To a solution of 2-chloropyridine-4-carbonitrile (20.0 g, 144 mmol) in 1-butanol (150 mL) was added 1 M solution of hydrazine hydrate in THF (303 mL, 303 mmol) dropwise at rt. It was then heated at 60° C. overnight. The mixture was concentrated, and the residue was purified by flash column chromatography (CH2Cl2/MeOH=20/1) to afford the title compound (3.5 g, 18%) as a white solid. [M+H] Calc'd for C6H6N4, 135. Found, 135.

후처리

  1. concentrationThe mixture was concentrated
  2. customthe residue was purified by flash column chromatography (CH2Cl2/MeOH=20/1)

출처 및 근거

ORD 기록
ord-26ee47ec087e4b198265ccbb98f6a1de
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09107916B2

연결된 노트

불러오는 중…