تفاعل #86613

معادلة التفاعل

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

HCl

diethyl ether

ammonia

→

title compound

المردود 100.0%

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

المردود 100.0%

المذيبات

methylene chloride

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution was cooled to 0° C.
2. 2
   أخرىgiving an immediate white precipitate
3. 3
   workup.WAITAfter 30 minutes
4. 4
   ترشيحthe slurry was filtered
5. 5
   ترشيحthe flask and filter cake
6. 6
   غسيلwere rinsed with methylene chloride (68 mL)
7. 7
   تركيزThe filtrate was concentrated

الإجراء التجريبي

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.

المصدر