反応 #1483099

反応方程式

mono methyl amine

59

dodecyl 2-bromopropanoate

sodium bicarbonate

→

60

収率 82.3%

dodecyl 2-(methylamino)propanoate

収率 82.3%

溶媒

acetonitrile

反応条件

後処理

1. 1
   その他The solid obtained in the reaction mixture
2. 2
   ろ過was filtered under vacuum
3. 3
   濃縮The solvent was concentrated
4. 4
   workup.ADDITIONdiluted with ethyl acetate/water
5. 5
   workup.STIRRINGstirred for 15 minutes at 25-30° C
6. 6
   その他The aqueous and organic layers were separated
7. 7
   抽出the aqueous layer was extracted with ethyl acetate (2×10 mL)
8. 8
   洗浄The combined organic layers were washed with brine solution
9. 9
   乾燥dried over Na2SO4
10. 10
    濃縮concentrated under vacuum

実験手順

To a stirred solution of 59 (10 g, 31.2 mmol) in acetonitrile (20 mL) was added sodium bicarbonate (2.62 g, 31.2 mmol) and followed by mono methyl amine (40% in water) (30 mL, 3 vol) at 25-30° C. The reaction mixture was stirred for 3 hour at 25-30° C.; the reaction was monitored by TLC. The solid obtained in the reaction mixture was filtered under vacuum. The solvent was concentrated, diluted with ethyl acetate/water and stirred for 15 minutes at 25-30° C. The aqueous and organic layers were separated, and the aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic layers were washed with brine solution, dried over Na2SO4 and concentrated under vacuum to afford crude 60 (7 g, yield: 82.3%) as a liquid

出典