Phosphorus oxychloride → HCID 86698900, 화합물

HRID 2174478노트

반응식

HRID 2174478 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:13][CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)=[C:6]2[C:11]=1[NH:10][C:9](=O)[CH:8]=[CH:7]2.O=P(Cl)(Cl)[Cl:24].[Cl-].C([NH+](CC)CC)C>C(#N)C>[Cl:24][C:9]1[CH:8]=[CH:7][C:6]2[C:11](=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:13][CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[N:10]=1

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 12698378Triethylazanium chlorideHCID 67977592HCID 67977592, 화합물

생성물 1

HCID 86698900HCID 86698900, 화합물수율 100%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
120 °C

실험 절차

8-chloro-5-(2-(piperidin-1-yl)ethoxy)quinolin-2(1H)-one (275 mg, 0.9 mmol, 1 eq.) was placed in acetonitrile (2.3 mL) in the presence of POCl3 (418 μL, 4.5 mmol, 5 eq.) and triethylammonium chloride (1 g, 4.5 mmol, 5 eq.). The reaction mixture was stirred at 120° C. during 3 hours. The mixture was then concentrated under reduced pressure and, after adding water to the residue (5 mL), was stirred at room temperature during 30 minutes. Then the resulting precipitate was washed with water and filtered to give 2,8-dichloro-5-(2-(piperidin-1-yl)ethoxy)quinoline (228 mg, 100%).

후처리

  1. concentrationThe mixture was then concentrated under reduced pressure
  2. additionafter adding water to the residue (5 mL)
  3. stirringwas stirred at room temperature during 30 minutes
  4. washThen the resulting precipitate was washed with water
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-d1cffd39606d408eb8824885eac0bf71
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09061999B2

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