Dichloromethane → 5-Amino7-(2-methylpropyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one Hydrochloride

HRID 413838

Reaktionsgleichung

Reaktionsgleichung von HRID 413838
C([NH:8][N:9]1[C:15](=O)[CH2:14][C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[C:11]2[CH:21]=[CH:22][CH:23]=[CH:24][C:10]1=2)(OC(C)(C)C)=O.[C:25]([O-:28])([O-])=O.[Cs+].[Cs+].I[CH2:32][CH:33](C)[CH3:34].C(Cl)[Cl:37]>CN(C=O)C>[ClH:37].[NH2:8][N:9]1[C:25](=[O:28])[CH:14]([CH2:15][CH:33]([CH3:34])[CH3:32])[C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[C:11]2[CH:21]=[CH:22][CH:23]=[CH:24][C:10]1=2

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 10556Isobutyl iodideHCID 10796Cesium carbonateHCID 114935485-(N-Boc-amino)-5,7-dihydro-6H-dibez[b,d]azepin-6-one

Produkt 1

HCID 222883145-Amino7-(2-methylpropyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one Hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (0.2 g, 0.617 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (0.22 g, 0.678 mmol) and warmed to 60° C. To the reaction mixture was added 1-iodo-2-methylpropane (0.078 ml, 0.678 mmol) and stirring continued for 17 h. After cooling to 23° C. the mixture was diluted with CH2Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was purified by chromatography (SiO2, CHCl3/MeOH 9:1).

Aufarbeitung

  1. temperatureAfter cooling to 23° C. the mixture
  2. washwashed with several portions of brine
  3. dry with materialdried over Na2SO4
  4. customThe title compound was purified by chromatography (SiO2, CHCl3/MeOH 9:1)

Quellen und Nachweise

ORD-Eintrag
ord-1d593881df6a474499899875e530f386
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06569851B1

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