Propylamine hydrochloride → 6-Methoxy-1,5-naphthyridin-4-amine

HRID 456579

反応式

HRID 456579 の反応式
[CH3:1][O:2][C:3]1[N:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][CH:7]=[C:6]2OS(C(F)(F)F)(=O)=O.Cl.C([NH2:25])CC>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[N:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][CH:7]=[C:6]2[NH2:25]

参加物

4

反応物 2

HCID 11165Propylamine hydrochlorideHCID 112552656-Methoxy-1,5-naphthyridin-4-yl trifluoromethanesulfonate

生成物 1

HCID 114352366-Methoxy-1,5-naphthyridin-4-amine収率 91.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of triflate (b) (25 g, 81.2 mmol) and propylamine hydrochloride (47 g, 487 mmol) in pyridine (300 ml) was heated to reflux overnight. The mixture was evaporated to dryness, dissolved in 0.5M aqueous hydrochloric acid (400 ml) and extracted three times with dichloromethane. The aqueous phase was then basified with 40% aqueous sodium hydroxide solution and extracted twice with dichloromethane. Drying and evaporation afforded a buff coloured solid (13.0 g, 90%).

後処理

  1. temperaturewas heated
  2. temperatureto reflux overnight
  3. customThe mixture was evaporated to dryness
  4. dissolutiondissolved in 0.5M aqueous hydrochloric acid (400 ml)
  5. extractionextracted three times with dichloromethane
  6. extractionextracted twice with dichloromethane
  7. customDrying
  8. customevaporation

出典と根拠

ORDレコード
ord-3162b2c3d3954e30bf5f676d9b6d0ff6
出典データセット
uspto-grants-2007_03
特許番号
US07186730B2

関連ノート

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