반응 #1483087

반응 방정식

DDAIP

4

dodecyl 2-(dimethylamino)propanoate

phosphoric acid

→

dodecyl 2-(dimethylamino)propanoate phosphorate salt

수율 93.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONAfter addition
2. 2
   농축The reaction mixture was concentrated under vacuum
3. 3
   workup.STIRRINGstirred at RT for 2 h

실험 절차

A stirred solution of DDAIP base 4 (100 g, 350 mmol) in ethyl acetate (500 mL) was cooled to 0° C. and then phosphoric acid 12 (34.38 g, 350 mmol) was added in one lot. After addition, the temperature of the reaction mixture was slowly raised to RT and stirred at RT for 12 h; the reaction mixture was monitored by TLC. The reaction mixture was concentrated under vacuum. The obtained sticky solid was taken in n-hexane (200 mL) and stirred at RT for 2 h to afford dodecyl 2-(dimethylamino)propanoate phosphorate salt (13, Nex-15) (125 g, 93%) as a sticky solid. 1H-NMR (400 MHz, CDCl3): δ 0.85 (t, 3H), 1.2-1.4 (m, 18H), 1.55 (d, 3H), 1.7 (q, 2H), 2.85 (s, 6H), 4.1 (q, 1H), 4.2 (t, 2H); LCMS: 286 (M++1); HPLC: 95.8%.

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