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

HRID 59598

反応式

HRID 59598 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

An 8 mL scintillation vial was charged with NiCl2.6H2O (12.0 mg, 0.051 mmol) and 2,2′-bipyridine (17.0 mg, 0.109 mmol). The vial was closed and purged with nitrogen for 5 min, after which the vial was charged with DMF (4.5 mL) and isopropyl alcohol (iPrOH; 0.5 mL). The mixture was allowed to stir for 5 min. To the vial was added zinc dust (0.2194 g, 3.4 mmol), and the mixture was allowed to stir under nitrogen for 35 min. Solid 3,4,5,6-tetrachloropicolinic acid (0.1076 g, 0.4 mmol) was added through the top of the reactor. The reaction mixture was allowed to stir at 14° C. 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 vial was closed
  2. custompurged with nitrogen for 5 min
  3. additionafter which the vial was charged with DMF (4.5 mL) and isopropyl alcohol (iPrOH; 0.5 mL)
  4. stirringto stir under nitrogen for 35 min
  5. stirringto stir at 14° C.
  6. customsamples were removed periodically
  7. customreaction kinetics

出典と根拠

ORDレコード
ord-24652201abc24b9a8a16feb899d600d6
出典データセット
uspto-grants-2016_09
特許番号
US09440923B2

関連ノート

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