Dimethylamine → HCID 76281363、化合物

反応式

Br[CH:2]([CH3:20])[C:3]([O:5][C:6]([CH3:19])([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH3:7])=[O:4].C(=O)(O)[O-].[Na+].[CH3:26][NH:27][CH3:28]>C(#N)C>[CH3:26][N:27]([CH3:28])[CH:2]([CH3:20])[C:3]([O:5][C:6]([CH3:19])([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH3:7])=[O:4]

参加物

反応条件

温度: 27.5 °C

実験手順

To a stirred solution of 74 (2 g, 5.7 mmol) in acetonitrile (10 mL) was added sodium bicarbonate (0.48 g, 5.74 mmol) and followed by dimethyl amine (40% in water) (10 mL, 88.8 mmol) at 25-30° C. The reaction mixture was stirred for 3 hours 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. The organic layer was dried over Na2SO4 and concentrated under vacuum to afford crude 75 (1.49 g, yield: 83%) as a liquid.