Hydrazine → 3,5-Dichloro-2-hydrazinylpyridine

HRID 453070ノート

反応式

HRID 453070 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 6009663,5-Dichloro-2-hydrazinylpyridine収率 72%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-77228aae130a4fbbaf2bddb21c1687bb
出典データセット
uspto-grants-2013_07
特許番号
US08492409B2

反応ノート

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