Hydrazine → HCID 178509226、化合物

HRID 390532ノート

反応式

HRID 390532 の反応式
Cl[C:2]1[C:7]([C:8]#[N:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:10][NH2:11].O1CCOCC1>C(OCC)(=O)C>[NH:10]1[C:2]2=[N:3][CH:4]=[CH:5][CH:6]=[C:7]2[C:8]([NH2:9])=[N:11]1

参加物

5

反応物 3

HCID 9321HydrazineHCID 312751,4-DioxaneHCID 810792-Chloronicotinonitrile

生成物 1

HCID 178509226HCID 178509226、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
150 °C

実験手順

2-Chloro-3-cyanopyridine (2.77 g), hydrazine (5 mL), and dioxane (100 mL) were combined in a sealed tube and heated at 150° C. for 16 hr. The reaction mixture was cooled to room temperature and concentrated in vacuo to provide a crude residue. The resultant residue was dissolved in ethyl acetate (100 mL) and washed with saturated NaCl solution (50 mL). The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo to afford 1H-pyrazolo[3,4-b]pyridin-3-ylamine as a yellow solid which was used without further purification.

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated in vacuo
  3. customto provide a crude residue
  4. washwashed with saturated NaCl solution (50 mL)
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0d57d7b0e1ae4d30934a9502f610a4bd
出典データセット
uspto-grants-2013_02
特許番号
US08383630B2

反応ノート

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