Hydrazine hydrate (1:1) → 2-Hydrazinyl-3-iodo-4-methylpyridine

HRID 2096986노트

반응식

HRID 2096986 반응식
Cl[C:2]1[C:7]([I:8])=[C:6]([CH3:9])[CH:5]=[CH:4][N:3]=1.O.[NH2:11][NH2:12]>N1C=CC=CC=1>[NH:11]([C:2]1[C:7]([I:8])=[C:6]([CH3:9])[CH:5]=[CH:4][N:3]=1)[NH2:12]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 451082072-Chloro-3-iodo-4-methylpyridine

생성물 1

HCID 581543012-Hydrazinyl-3-iodo-4-methylpyridine수율 87%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 2-chloro-3-iodo-4-methylpyridine (preparation 28a, 2.0 g, 7.9 mmol) and hydrazine hydrate (1.2 mL, 24.2 mmol) in pyridine (12 mL) under an argon atmosphere was stirred and heated to reflux. After 24 hours, the mixture was cooled and evaporated to dryness. The crude mixture was triturated with water and the solid was filtered and washed with water to give the title compound (1.71 g, 87%) which was used without further purification in the next reaction.

후처리

  1. temperatureheated to reflux
  2. temperaturethe mixture was cooled
  3. customevaporated to dryness
  4. customThe crude mixture was triturated with water
  5. filtrationthe solid was filtered
  6. washwashed with water

출처 및 근거

ORD 기록
ord-a29fe50d7b4c424f8c8843fbd62557c8
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450341B2

반응 노트

불러오는 중…