Dichloromethane → HCID 10382997, Verbindung

HRID 1352495Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1352495
[CH3:1][CH:2]1[CH2:11][CH:10]([NH:12][CH2:13][C:14]#[CH:15])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]1[C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:17].C(N([CH:30]([CH3:32])C)CC)(C)C.ClCCl.C(=O)([O-])[O-:37].[K+].[K+]>O1CCOCC1>[C:16]([N:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:10]([N:12]([CH2:13][C:14]#[CH:15])[C:30](=[O:37])[CH3:32])[CH2:11][CH:2]1[CH3:1])(=[O:17])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 22935713HCID 22935713, Verbindung

Produkt 1

HCID 10382997HCID 10382997, VerbindungAusbeute 58,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of (2-methyl-4-prop-2-ynylamino-3,4-dihydro-2H-quinolin-1-yl)-phenyl-methanone (0.06 g), diisopropyl ethyl amine (0.038 g) in dioxane (5 ml), anhydride acetic (0.2 g) was added under stirring. The mixture was heated under reflux over the night. After cooling dichloromethane and an aqueous solution of potassium carbonate were added. The organic layer was separated, and then dried over sodium sulfate. Organic solvent was removed under reduce pressure to give the crude compound (0.15 g). Purification by chromatography was performed with dichloromethane/methanol (99/1) as eluent to give the desired title compound (0.04 g, 58.8% yield).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux over the night
  3. customThe organic layer was separated
  4. dry with materialdried over sodium sulfate
  5. customOrganic solvent was removed
  6. customto give the crude compound (0.15 g)
  7. customPurification by chromatography

Quellen und Nachweise

ORD-Eintrag
ord-794b2bf971e7467ca02c7291e8721d69
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07220760B2

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