Triethylamine → Methanesulfonamide,n-[3-[(4-chloro-2,3-dihydro-7-iodo-1-oxo-1h-isoindol-5-yl)oxy]propyl]-

HRID 21315Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 21315
Cl.[Cl:2][C:3]1[C:11]([O:12][CH2:13][CH2:14][CH2:15][NH2:16])=[CH:10][C:9]([I:17])=[C:8]2[C:4]=1[CH2:5][NH:6][C:7]2=[O:18].C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>ClCCl>[Cl:2][C:3]1[C:11]([O:12][CH2:13][CH2:14][CH2:15][NH:16][S:27]([CH3:26])(=[O:29])=[O:28])=[CH:10][C:9]([I:17])=[C:8]2[C:4]=1[CH2:5][NH:6][C:7]2=[O:18]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 684884094-Chloro-5-(3-aminopropoxy)-7-iodoisoindolinone hydrochloride

Produkt 1

HCID 68492844Methanesulfonamide,n-[3-[(4-chloro-2,3-dihydro-7-iodo-1-oxo-1h-isoindol-5-yl)oxy]propyl]-Ausbeute 47 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

4-Chloro-5-(3-aminopropoxy)-7-iodoisoindolinone hydrochloride (100 mg, 0.248 mmol) was suspended in dichloromethane (3.0 mL), and the suspension was added with triethylamine (0.104 mL, 0.744 mmol) and methanesulfonyl chloride (0.029 mL, 0.372 mmol), followed by stirring at room temperature for 13 hours. The solvent was evaporated under reduced pressure, and the residue was purified by slurry using water and acetonitrile to obtain 4-chloro-5-[3-(methanesulfonylamino)propoxy]-7-iodoisoindolinone (51.8 mg, yield 47%).

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by slurry

Quellen und Nachweise

ORD-Eintrag
ord-38d0b3e4e8f44f649fd85c9b6ec23f7d
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07745641B2

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