Hydrazine hydrate (1:1) → 4-(4-Chlorophenyl)-2-hydrazinyl-3,4'-bipyridine

HRID 2101316

반응식

HRID 2101316 반응식
Cl[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)=[C:6]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[CH:5]=[CH:4][N:3]=1.O.[NH2:22][NH2:23]>N1C=CC=CC=1>[Cl:20][C:17]1[CH:18]=[CH:19][C:14]([C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH:22][NH2:23])[C:7]=2[C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)=[CH:15][CH:16]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 577993632-Chloro-4-(4-chlorophenyl)-3,4'-bipyridine

생성물 1

HCID 577994604-(4-Chlorophenyl)-2-hydrazinyl-3,4'-bipyridine수율 78.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a stirring solution of 2-chloro-4-(4-chlorophenyl)-3,4′-bipyridine (1.3 g, 4.3 mmol) in pyridine (5 mL) at room temperature under argon was added hydrazine monohydrate (2.5 mL, 51.5 mmol). The reaction mixture was stirred at reflux under argon for 15 h. After cooling the reaction mixture to room temperature, most of the solvent was removed under reduced pressure. Water (25 mL) was added to the residue while stirring and a precipitate formed. The precipitate was collected by filtration and washed with water (15 mL×2). After drying under reduced pressure at elevated temperature, 1.0 g of the title compound was obtained as a yellow solid. HPLC/MS: retention time=1.68 min, [M+H]+=297.

후처리

  1. temperatureat reflux under argon for 15 h
  2. custommost of the solvent was removed under reduced pressure
  3. additionWater (25 mL) was added to the residue
  4. stirringwhile stirring
  5. customa precipitate formed
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water (15 mL×2)
  8. customAfter drying under reduced pressure at elevated temperature

출처 및 근거

ORD 기록
ord-9ee2c7577d5a455c859b9b5cbe713725
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572808B2

연결된 노트

불러오는 중…