Sodium Carbonate → HCID 22024220, 화합물

HRID 1792753노트

반응식

HRID 1792753 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 22024220HCID 22024220, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-7b93615a1aee4f05861c3a6bb484f95d
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07078403B1

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