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

HRID 1434636

反応式

HRID 1434636 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 218827665-Iodopyridine-2,3-diamine収率 60%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4a27429fc4e14527be8693d1c860e8c4
出典データセット
uspto-grants-2009_11
特許番号
US07615567B2

関連ノート

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