2,2'-Bipyridine → 2-Pyridinecarboxylic acid, 4,5,6-trichloro-

HRID 59599

反応式

HRID 59599 の反応式
N1C=CC=CC=1C1C=CC=CN=1.Cl[C:14]1[C:15]([C:23]([OH:25])=[O:24])=[N:16][C:17]([Cl:22])=[C:18]([Cl:21])[C:19]=1[Cl:20]>[Zn].C(#N)C>[Cl:20][C:19]1[C:18]([Cl:21])=[C:17]([Cl:22])[N:16]=[C:15]([C:23]([OH:25])=[O:24])[CH:14]=1

参加物

5

反応物 2

HCID 14742,2'-BipyridineHCID 826463,4,5,6-Tetrachloropyridine-2-carboxylic acid

生成物 1

HCID 129936922-Pyridinecarboxylic acid, 4,5,6-trichloro-

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 6342Acetonitrile溶媒

実験手順

Three 8 mL scintillation vials were charged with NiCl2.6H2O (12.0 mg, 0.051 mmol) and 2,2′-bipyridine (16.0 mg, 0.102 mmol). The vials were closed and purged with nitrogen for 5 min, after which the vials were charged with DMF (4.5 mL) and one of the following: deionized (DI) water (pH=7), 10% HCl, or 10% sodium hydroxide (NaOH) (0.5 mL). The mixtures were allowed to stir for 5 min. To each of the vials was added zinc dust (0.22 g, 3.4 mmol), and the mixtures were allowed to stir under nitrogen for 35 min. Solid 3,4,5,6-tetrachloropicolinic acid (0.10 g, 0.4 mmol) was added to each through the top of the reactor. The reaction mixtures were allowed to stir at ambient temperature, and samples were removed periodically to determine reaction kinetics. The samples (˜0.01 mL of reaction mixture diluted to 1.5 mL with acetonitrile) were analyzed by a calibrated HPLC method.

後処理

  1. customThe vials were closed
  2. custompurged with nitrogen for 5 min
  3. additionafter which the vials were charged with DMF (4.5 mL) and one of the following:
  4. stirringto stir under nitrogen for 35 min
  5. customThe reaction mixtures
  6. stirringto stir at ambient temperature
  7. customsamples were removed periodically
  8. customreaction kinetics

出典と根拠

ORDレコード
ord-475aa84afd6c442bb689109156402f42
出典データセット
uspto-grants-2016_09
特許番号
US09440923B2

関連ノート

読み込み中…