반응 #86613

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N2-(tert-butoxycarbonyl)-N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride

HCl

diethyl ether

ammonia

→

title compound

수율 100.0%

N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride

수율 100.0%

용매

methylene chloride

methanol

methanol

반응 조건

후처리

1. 1
   온도The solution was cooled to 0° C.
2. 2
   기타giving an immediate white precipitate
3. 3
   workup.WAITAfter 30 minutes
4. 4
   여과the slurry was filtered
5. 5
   여과the flask and filter cake
6. 6
   세척were rinsed with methylene chloride (68 mL)
7. 7
   농축The filtrate was concentrated

실험 절차

To a solution of N2-(tert-butoxycarbonyl)-N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride (7.6 g, 14 mol) in methylene chloride (38 mL) and methanol (4.2 mL) was added 2.0 M HCl in diethyl ether (16 mL, 32 mmol), and the mixture was stirred overnight at room temperature. The solution was cooled to 0° C. and treated with 7 M ammonia in methanol (6.0 mL, 42 mmol), giving an immediate white precipitate. After 30 minutes, the slurry was filtered and the flask and filter cake were rinsed with methylene chloride (68 mL). The filtrate was concentrated to give the title compound (6.2 g, 100%) as a crude white solid.

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