Water → 6-Chloro-3-hydrazinyl-4-methylpyridazine

HRID 874013

반응식

HRID 874013 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[CH3:8].O.[NH2:11][NH2:12].O>CCO>[Cl:9][C:5]1[N:4]=[N:3][C:2]([NH:11][NH2:12])=[C:7]([CH3:8])[CH:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 879233,6-Dichloro-4-methylpyridazine

생성물 1

HCID 114464906-Chloro-3-hydrazinyl-4-methylpyridazine수율 39.1%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

3,6-Dichloro-4-methylpyridazine (Combi-Blocks) (60 g, 361 mmol) was dissolved in hydrazine monohydrate (Aldrich) (335 mL, 5411 mmol) and the solution was stirred at 80° C. for 1 h, forming a white precipitate. The reaction mixture is dilutes with water and the precipitated products isolated by filtration. The solid crude product is suspended in EtOH and left in an ultra sound bath for 1 h. The desired product (22.4 g) was obtained after filtration and drying under vacuum as a beige solid. tR: 0.31 min (LC-MS 2); ESI-MS: 160.0 [M+H]+ (LC-MS 2). 1H NMR (400 MHz; DMSO-d6) δ ppm 7.83 (br.s, 1H) 7.32 (s, 1H) 4.49 (br.s, 2H) 2.05 (s, 3H).

후처리

  1. customforming a white precipitate
  2. customthe precipitated products isolated by filtration
  3. waitleft in an ultra sound bath for 1 h

출처 및 근거

ORD 기록
ord-cb3edca2b4dd4f3fab854d9cc4acc786
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975417B2

연결된 노트

불러오는 중…