반응 #86622

반응 방정식

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

수율 98.1%

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

수율 98.1%

용매

methanol

methanol

methylene chloride

반응 조건

후처리

1. 1
   온도cooled with an ice bath
2. 2
   workup.WAITAfter 30 minutes
3. 3
   기타the slurry that resulted
4. 4
   여과was filtered
5. 5
   세척the solids were washed with methylene chloride
6. 6
   농축The filtrate was concentrated

실험 절차

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.

출처