Sodium Carbonate → HCID 22024220、化合物

HRID 1792753ノート

反応式

HRID 1792753 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][OH:7].Cl[C:9]1[CH:14]=[CH:13][N:12]=[N:11][C:10]=1[Cl:15].C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1>[Cl:15][C:10]1[N:11]=[N:12][C:13]([NH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][OH:7])=[CH:14][CH:9]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 756345-Aminopentan-1-olHCID 2521503,4-dichloropyridazine

生成物 1

HCID 22024220HCID 22024220、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 5-amino-1-pentanol (433 mg, 4.2 mmol), dichloropyridazine (1.25 g, 8.39 mmol) and sodium carbonate (890 mg, 8.39 mmol) was stirred in 1,4-dioxane (40 ml) and heated at 70-80° for 3 days under an atmosphere of argon. The solvent was removed under reduced pressure and the residue was partitioned between dichloromethane (300 ml) and water (38 ml). The organic layer was separated, dried and concentrated to give an orange solid which was chromatographed on silica, using hexane/ethyl acetate (1:1). The product, 5-(6chloro-3-pyridazinyl)amino-1-pentanol was isolated as a pale yellow solid (202 mg, 22%).

後処理

  1. temperatureheated at 70-80° for 3 days under an atmosphere of argon
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was partitioned between dichloromethane (300 ml) and water (38 ml)
  4. customThe organic layer was separated
  5. customdried
  6. concentrationconcentrated
  7. customto give an orange solid which
  8. customwas chromatographed on silica

出典と根拠

ORDレコード
ord-7b93615a1aee4f05861c3a6bb484f95d
出典データセット
uspto-grants-2006_07
特許番号
US07078403B1

反応ノート

読み込み中…