Reaktion #86622

Reaktionsgleichung

hydrogen chloride

diethyl ether

ammonia

8,8,11,14,14-pentamethyl-7,12-dioxo-1,1,1-triphenyl-13-oxa-6,11-diaza-1-phosphoniapentadecane bromide

→

title compound

Ausbeute 98.1%

(4-{[2,2-dimethyl-4-(methylamino)butanoyl]amino}butyl)(triphenyl)phosphonium bromide

Ausbeute 98.1%

Lösungsmittel

methanol

methanol

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled with an ice bath
2. 2
   workup.WAITAfter 30 minutes
3. 3
   Sonstigethe slurry that resulted
4. 4
   Filtrationwas filtered
5. 5
   Waschenthe solids were washed with methylene chloride
6. 6
   EinengenThe filtrate was concentrated

Vorschrift

8,8,11,14,14-pentamethyl-7,12-dioxo-1,1,1-triphenyl-13-oxa-6,11-diaza-1-phosphoniapentadecane bromide (205 mg, 0.32 mmol) was dissolved in methylene chloride (1.0 mL) and methanol (0.10 mL). The solution at room temperature was treated with 2.0 M hydrogen chloride in diethyl ether (0.36 mL, 0.71 mmol). The reaction was stirred overnight at room temperature, cooled with an ice bath, and treated with 7N ammonia in methanol (0.13 mL, 0.93 mmol). After 30 minutes, the slurry that resulted was filtered, and the solids were washed with methylene chloride. The filtrate was concentrated to give the title compound (170 mg, 98%) as a white foam. The product of step 2 was used crude in next step.

Quelle