Hydrochloric Acid → 2,6-Dichloropyridine-3,4-diamine

HRID 57516

반응식

HRID 57516 반응식
[Cl:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([NH2:11])[CH:5]=[C:4]([Cl:12])[N:3]=1.O.Cl>C(O)C.[Fe]>[Cl:1][C:2]1[C:7]([NH2:8])=[C:6]([NH2:11])[CH:5]=[C:4]([Cl:12])[N:3]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 2827402,6-Dichloro-3-nitropyridin-4-amine

생성물 1

HCID 109319872,6-Dichloropyridine-3,4-diamine수율 86.5%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

반응 조건

온도
95 °C

실험 절차

To a solution of 2,6-dichloro-3-nitropyridin-4-amine in ethanol (150 mL) was added iron powder (14.3 g, 0.255 mol), water (46 mL), and then concentrated HCl (28 mL). The reaction mixture was then stirred at 95° C. for 16 hours, cooled to room temperature, and neutralized. The precipitates were collected by filtration and dried in vacuo. The crude product was then treated with water (200 mL) and extracted with EtOAc (3×200 mL). The combined extracts were dried over anhydrous Na2SO4, filtered, and concentrated to afford 7.85 g of the title compound (86.5% yield).

후처리

  1. temperaturecooled to room temperature
  2. filtrationThe precipitates were collected by filtration
  3. customdried in vacuo
  4. additionThe crude product was then treated with water (200 mL)
  5. extractionextracted with EtOAc (3×200 mL)
  6. dry with materialThe combined extracts were dried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e7a3ccedbad14f8e928c8f02d0d5d9a6
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434726B2

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