Hydrazine → 3,5-Dichloro-2-hydrazinylpyridine

HRID 453070

반응식

HRID 453070 반응식
Cl[C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.[NH2:10][NH2:11]>O1CCOCC1>[Cl:8][C:7]1[C:2]([NH:10][NH2:11])=[N:3][CH:4]=[C:5]([Cl:9])[CH:6]=1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 27666Pyridine, 2,3,5-trichloro-

생성물 1

HCID 6009663,5-Dichloro-2-hydrazinylpyridine수율 72%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a 500 mL flask, 2,3,5-trichloropyridine (20.00 g, 0.110 mol), 80% hydrazine (34.30 g, 0.550 mol) and dioxane (200 mL) were added sequentially. The reaction mixture was heated to reflux for 20 hours. Then the reaction mixture was cooled down to room temperature overnight and white crystal was precipitated. The white crystal was isolated via filtration and dried to give the product (14.0 g) as a white solid in 72% yield. Melting point: 187-189° C. 1H NMR (300 MHz, DMSO-d6): 8.123 (d, 1H), 7.849 (d, 1H).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 20 hours
  3. customwhite crystal was precipitated
  4. customThe white crystal was isolated via filtration
  5. customdried

출처 및 근거

ORD 기록
ord-77228aae130a4fbbaf2bddb21c1687bb
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492409B2

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