Hydrochloric Acid → 5,6-Diphenyl-pyridine-2-carboxylic acid

HRID 12565

反応式

HRID 12565 の反応式
[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([C:19]([O:21]CC)=[O:20])=[N:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Li+].[OH-].Cl>CCO>[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([C:19]([OH:21])=[O:20])=[N:11][C:12]=2[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 14789610Ethyl 5,6-diphenylpyridine-2-carboxylate2 回

生成物 1

HCID 214715265,6-Diphenyl-pyridine-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of ethyl 5,6-diphenylpyridine-2-carboxylate (Compound 21, 40 mg, 0.13 mmol) and LiOH (1N, 1 ml) in EtOH (2 ml) was stirred at room temperature overnight. The mixture was acidified with 10% HCl, then extracted with EtOAc. The organic layer was washed with water, and brine, and dried over Na2SO4. The filtered solvent was concentrated in vacuo, and the residue was purified by silica gel chromatography (20-80% Ethyl acetate in hexane) to give title compound as a solid.

後処理

  1. extractionextracted with EtOAc
  2. washThe organic layer was washed with water, and brine
  3. dry with materialdried over Na2SO4
  4. concentrationThe filtered solvent was concentrated in vacuo
  5. customthe residue was purified by silica gel chromatography (20-80% Ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-43af859442634bd7bb2952e0d4381809
出典データセット
uspto-grants-2010_06
特許番号
US07728014B2

関連ノート

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