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

HRID 977053노트

반응식

HRID 977053 반응식
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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 784Hydrogen Peroxide2회HCID 10340Sodium CarbonateHCID 118508274,5-dichloropyridin-3-amine

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a45155736f554726b5898512c4b1239a
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05614469

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