Trifluoroacetic acid → (RS)-7-Amino-5H,7H-dibenzo[b,d]azepin-6-one

HRID 1372941Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1372941
[NH2:1][CH:2]1[C:8](=[O:9])[N:7](CC2C=CC(OC)=CC=2)[C:6]2[CH:19]=[CH:20][CH:21]=[CH:22][C:5]=2[C:4]2[CH:23]=[CH:24][CH:25]=[CH:26][C:3]1=2.FC(F)(F)C(O)=O.FC(F)(F)S(O)(=O)=O.C([O-])(O)=O.[Na+]>ClCCl>[NH2:1][CH:2]1[C:8](=[O:9])[NH:7][C:6]2[CH:19]=[CH:20][CH:21]=[CH:22][C:5]=2[C:4]2[CH:23]=[CH:24][CH:25]=[CH:26][C:3]1=2

Komponenten

6

Edukt 4

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 516892Sodium BicarbonateHCID 210725617-Amino-5-(4-methoxybenzyl)-5,7-dihydro-6H-dibenzo[b,d]azepin-6-one

Produkt 1

HCID 23555091(RS)-7-Amino-5H,7H-dibenzo[b,d]azepin-6-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 0.1 g (0.29 mmol) (RS)-7-amino-5-(4-methoxy-benzyl)-5H,7H-dibenzo[b,d]azepin-6-one in 8 ml of dichloromethane at 0° C. temperature 0.67 ml (8.7 mmol) of trifluoroacetic acid and 0.25 ml of trifluoromethansulfonic acid (2.9 mmol) were added and the mixture was stirred for 4 hours at room temperature. After concentration of the mixture at 40° C. in vacuo an aqueous NaHCO3 solution was added and the mixture extracted two times with ethyl acetate. The combined organic layers were dried (MgSO4). After evaporation of the solvent a light yellow oil was obtained, that was used directly in the next step.

Aufarbeitung

  1. extractionthe mixture extracted two times with ethyl acetate
  2. dry with materialThe combined organic layers were dried (MgSO4)
  3. customAfter evaporation of the solvent a light yellow oil
  4. customwas obtained

Quellen und Nachweise

ORD-Eintrag
ord-904d55d679ab4a42a07d64ff57a9ce26
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07160875B2

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