Dimethyl Sulfoxide → n-Pyridin-2-yl-n-(pyridin-2-ylmethyl)pyridin-2-amine

HRID 1970732

反応式

HRID 1970732 の反応式
[OH-].[K+].CS(C)=O.[CH:7]1[CH:12]=[C:11]([NH:13][C:14]2[N:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:10]=[CH:9][CH:8]=1.Cl.Cl[CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=1>O>[N:19]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[N:13]([CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=1)[C:11]1[CH:12]=[CH:7][CH:8]=[CH:9][N:10]=1

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 145472,2'-DipyridylamineHCID 14797Potassium HydroxideHCID 23392Picolyl chloride hydrochloride

生成物 1

HCID 15554506n-Pyridin-2-yl-n-(pyridin-2-ylmethyl)pyridin-2-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a flask were added 5.2 g pulverized potassium hydroxide and 35 ml dimethylsulfoxide. After adding 3.4 g 2,2′-dipyridylamine, the mixture was stirred under nitrogen for 45 minutes, when 3.3 g 2-(chloromethyl)pyridine hydrochloride was added. After stirring for 1 hour, 100 ml of water was added and the product was extracted with 60 ml of 50% ethyl acetate, 50% hexane. The organic layer was washed with 30 ml water and the solvent was removed. The residue was added to 5 ml hot ethanol, and 20 ml of water was added.

後処理

  1. additionTo a flask were added 5.2 g
  2. stirringAfter stirring for 1 hour
  3. extractionthe product was extracted with 60 ml of 50% ethyl acetate, 50% hexane
  4. washThe organic layer was washed with 30 ml water
  5. customthe solvent was removed
  6. additionThe residue was added to 5 ml hot ethanol, and 20 ml of water
  7. additionwas added

出典と根拠

ORDレコード
ord-bb3395e099734450abe6fdf92e6f9ada
出典データセット
uspto-grants-2013_04
特許番号
US08431045B2

関連ノート

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