Hydrochloric Acid → 2,4,5-Trichloropyridin-3-amine

HRID 2211006ノート

反応式

HRID 2211006 の反応式
OO.[NH2:3][C:4]1[CH:5]=[N:6][CH:7]=[C:8]([Cl:11])[C:9]=1[Cl:10].C(=O)([O-])[O-].[Na+].[Na+].[ClH:18]>O>[NH2:3][C:4]1[C:5]([Cl:18])=[N:6][CH:7]=[C:8]([Cl:11])[C:9]=1[Cl:10]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 784Hydrogen Peroxide2 回HCID 10340Sodium CarbonateHCID 118508274,5-dichloropyridin-3-amine

生成物 1

HCID 214644352,4,5-Trichloropyridin-3-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Thirty percent aqueous hydrogen peroxide (3.0 g, 26 mmole) was added dropwise with stirring at 15° C. to a solution of 8.0 g (49 mmol) of 3-amino-4,5-dichloropyridine in 450 mL of 37 percent aqueous hydrochloric acid. After 30 min another 2.6 g (23 mmol) of 30 percent aqueous hydrogen peroxide was added and the solution was allowed to slowly warm to room temperature. The resulting mixture was diluted with water, neutralized with sodium carbonate, and extracted with ether. The ethereal extract was dried over magnesium sulfate and filtered. The filtrate was concentrated by evaporation under reduced pressure to obtain a viscous oil. This oil was partially purified by column chromatography to obtain 2.5 g (26 percent of theory) of the title compound, a white solid melting at 88°-90° C., and 5.3 g of a mixture of the title compound and 3-amino-2,4,5,6-tetrachloropyridine.

後処理

  1. extractionextracted with ether
  2. extractionThe ethereal extract
  3. dry with materialwas dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  6. customto obtain a viscous oil
  7. customThis oil was partially purified by column chromatography

出典と根拠

ORDレコード
ord-681c77f961254cb6a84506389ceed1cc
出典データセット
uspto-grants-1995_10
特許番号
US05461161

反応ノート

読み込み中…