2-Amino-3-nitro-6-(phenylmercapto)pyridine → 2,3-Diamino-6-(phenylmercapto)pyridine

HRID 2289499ノート

反応式

HRID 2289499 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][CH:5]=[C:4]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:3]=1.[H][H]>CC(O)C.[Ni]>[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[C:4]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:3]=1

参加物

5

反応物 2

HCID 110212152-Amino-3-nitro-6-(phenylmercapto)pyridineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 110638822,3-Diamino-6-(phenylmercapto)pyridine収率 87.1%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 3776Isopropanol溶媒

実験手順

2,3-Diamino-6-(phenylmercapto)pyridine was prepared by hydrogenating 2-amino-3-nitro-6-(phenylmercapto)pyridine (107.1 g, 0.433 mol) under 5 atm of H2 in the presence of 30 g of Raney-Ni in 1200 mL of 2-propanol at 70° C. After 4 hours (29.1 L of hydrogen) the reaction mixture was cooled to 4° C. while stirring continuously. The precipitate was collected by vacuum filtration, washed with 2-propanol and dried at 50° C. under vacuum. The combined filtrates were concentrated under reduced pressure and recrystallized from 2-propanol. After washing the hydrogenation apparatus twice with 1000 mL of THF, evaporation under reduced pressure and recrystallization from 2-propanol, the precipitate was collected and dried at 50° C. under vacuum to give 80.4 g (87.1% yield) of 2,3-diamino-6-(phenylmercapto)pyridine m.p. 119-122° C.)

後処理

  1. filtrationThe precipitate was collected by vacuum filtration
  2. washwashed with 2-propanol
  3. customdried at 50° C. under vacuum
  4. concentrationThe combined filtrates were concentrated under reduced pressure
  5. customrecrystallized from 2-propanol
  6. washAfter washing the hydrogenation apparatus
  7. customtwice with 1000 mL of THF, evaporation
  8. customunder reduced pressure and recrystallization from 2-propanol
  9. customthe precipitate was collected
  10. customdried at 50° C. under vacuum

出典と根拠

ORDレコード
ord-e2e333ec207348b29bf194b309ee0ae4
出典データセット
uspto-grants-2000_07
特許番号
US06093728

反応ノート

読み込み中…