Hydrochloric Acid → 5-Iodopyridine-2,3-diamine

HRID 1434636

반응식

HRID 1434636 반응식
[I:1][C:2]1[CH:3]=[C:4]([N+:9]([O-])=O)[C:5]([NH2:8])=[N:6][CH:7]=1.C(O)C.Cl>[Fe].O>[I:1][C:2]1[CH:3]=[C:4]([NH2:9])[C:5]([NH2:8])=[N:6][CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 33844682-Amino-5-iodo-3-nitropyridine

생성물 1

HCID 218827665-Iodopyridine-2,3-diamine수율 60%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

5-Iodo-3-nitro-2-aminopyridine (2.0 g, 7.55 mmol), ethanol (7 mL), water (2 mL), and concentrated HCl (0.10 mL) were added to a 25 mL round bottom flask and allowed to stir. Iron (4.8 g, 85.9 mmol) was added in portions to the reaction followed by heating at 100° C. for 30 min. The iron was then removed and washed with ethanol over a flitted filter while the ethanol washings were concentrated under reduced pressure. The residue was purified by flash chromatography using 1:2 hexane:ethyl acetate as eluent to give 5-Iodo-2,3-diaminopyridine as a light brown solid (60%, 1.061 g).

후처리

  1. customThe iron was then removed
  2. washwashed with ethanol over
  3. filtrationa flitted filter while the ethanol washings
  4. concentrationwere concentrated under reduced pressure
  5. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-4a27429fc4e14527be8693d1c860e8c4
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07615567B2

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