Reaktion #807321

Reaktionsgleichung

title compound

1,1-Dimethylethyl (1R)-1-[(4-hydroxyphenyl)methyl]-2-oxo-2-[(6-oxo-2-phenyl-5,6-dihydro-1H-[1,2]diazepino[4,5,6-cd]indol-8-yl)amino]ethyl(methyl)carbamate

HCl

triethylamine

→

title compound

Ausbeute 48.0%

(2R)-3-(4-Hydroxyphenyl)-2-(methylamino)-N-(6-oxo-2-phenyl-5,6-dihydro-1H-[1,2]diazepino[4,5,6-cd]indol-8-yl)propanamide hydrochloride

Ausbeute 48.0%

Lösungsmittel

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Wascheneluting with 3:1:1 hexane
2. 2
   TemperaturWith ice bath cooling
3. 3
   workup.ADDITIONthe purified freebase in CH2Cl2 (10 mL) was treated with 4M HCl in dioxane (0.1 mL)
4. 4
   SonstigeAfter removal of the volatile components

Vorschrift

Preparation of example 167 from the title compound of Example 151 (47 mg, 0.085 mmol) and 4M HCl in dioxane (10 mL) was carried out analogously to Example 91. Isolation, also in an analogous manner, included freebasing with triethylamine and subsequent silica gel chromatography eluting with 3:1:1 hexane:ethyl acetate:ethanol. With ice bath cooling, the purified freebase in CH2Cl2 (10 mL) was treated with 4M HCl in dioxane (0.1 mL). After removal of the volatile components, the title compound (20 mg, 0.041 mmol) was obtained as an orange/yellow powder in 48% yield.

Quelle