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

HRID 977053ノート

反応式

HRID 977053 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 mmol) was added dropwise with stirring at 15° C. to a solution of 8.0 g (49mmol) of 3-amino-4,5-dichloropyridine in 450mL 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 liltrate 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 liltrate 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-a45155736f554726b5898512c4b1239a
出典データセット
uspto-grants-1997_03
特許番号
US05614469

反応ノート

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