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Trifluoroacetic acid → N-Cyclopropyl-3-fluoro-5-{2-(3-hydroxy-2,2-dimethylpropyl)-4-[(4-methyl-1,4-diazepan-1-yl)methyl]-1-oxo-1,2-dihydroisoquinolin-6-yl}-4-methylbenzamide

HRID 906407
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 906407
[CH:1]1([NH:4][C:5](=[O:33])[C:6]2[CH:11]=[C:10]([C:12]3[CH:13]=[C:14]4[C:19](=[CH:20][CH:21]=3)[C:18](=[O:22])[N:17]([CH2:23][C:24]([CH3:28])([CH3:27])[CH2:25][OH:26])[CH:16]=[C:15]4[CH:29]=O)[C:9]([CH3:31])=[C:8]([F:32])[CH:7]=2)[CH2:3][CH2:2]1.[CH3:34][N:35]1[CH2:41][CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(C(F)(F)F)=O>CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[CH:1]1([NH:4][C:5](=[O:33])[C:6]2[CH:11]=[C:10]([C:12]3[CH:13]=[C:14]4[C:19](=[CH:20][CH:21]=3)[C:18](=[O:22])[N:17]([CH2:23][C:24]([CH3:27])([CH3:28])[CH2:25][OH:26])[CH:16]=[C:15]4[CH2:29][N:38]3[CH2:39][CH2:40][CH2:41][N:35]([CH3:34])[CH2:36][CH2:37]3)[C:9]([CH3:31])=[C:8]([F:32])[CH:7]=2)[CH2:2][CH2:3]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6422Trifluoroacetic acidHCID 2283491-MethylhomopiperazineHCID 5049666Sodium triacetoxyborohydrideHCID 86640963N-Cyclopropyl-3-fluoro-5-(4-formyl-2-(3-hydroxy-2,2-dimethylpropyl)-1-oxo-1,2-dihydroisoquinolin-6-yl)-4-methylbenzamide

Produkt 1

HCID 59285293
N-Cyclopropyl-3-fluoro-5-{2-(3-hydroxy-2,2-dimethylpropyl)-4-[(4-methyl-1,4-diazepan-1-yl)methyl]-1-oxo-1,2-dihydroisoquinolin-6-yl}-4-methylbenzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 11026Titanium isopropoxideKatalysator

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

To a mixture of N-cyclopropyl-3-fluoro-5-(4-formyl-2-(3-hydroxy-2,2-dimethylpropyl)-1-oxo-1,2-dihydroisoquinolin-6-yl)-4-methylbenzamide (Example 2c, 0.20 g) and titanium(IV) isopropoxide (2 mL) was added 1-methyl-1,4-diazepane (0.17 mL) under nitrogen. The resulting mixture was stirred at 20° C. for 2 h before adding sodium triacetoxyborohydride (0.38 g). The mixture was stirred at room temperature for 2 h. TFA (5 mL) was added and the mixture stirred at room temperature for 72 h and then evaporated to dryness. The mixture was quenched with 10% aq ammonia (5 ml) and extracted with ethyl acetate. The organic was dried (MgSO4), filtered and evaporated to afford crude product. The crude product was purified by preparative HPLC (Phenomenex Gemini column using a 95-5% gradient of aqueous 0.2% ammonia in acetonitrile as eluent) to afford the title compound (0.055 g) as a white solid.

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for 2 h
  2. stirringthe mixture stirred at room temperature for 72 h
  3. customevaporated to dryness
  4. customThe mixture was quenched with 10% aq ammonia (5 ml)
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic was dried (MgSO4)
  7. filtrationfiltered
  8. customevaporated
  9. customto afford crude product
  10. customThe crude product was purified by preparative HPLC (Phenomenex Gemini column

Quellen und Nachweise

ORD-Eintrag
ord-e6452cc9dc664b428674b8002894718f
Quelldatensatz
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08012980B2

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