活性酮法制备酰胺

exanes:EtOAc); 1 HNMR (300 MHz, CDCl 3 ): δ 5.43 (m, 1H), 4.72 (s, 1H), 4.17-4.11 (m,1H), 3.71 (s, 3H), 3.22 (s, 3H), 2.59-2.24 (comp. m, 3H), 2.03 (dd, J =14.6 Hz, 4.1 Hz, 1H), 1.75-1.71 (m, 3H), 0.86 (s, 9H), 0.11 (s, 3H), 0.09 (s,3H).

三、苯甲硫酸乙酸还原吡啶下面

A mixture of the benzoicacid (10 mmol), 4-methylbenzene-1-sulfonyl chloride (10 mmol), K 2 CO 3 (5.52 g, 40 mmol) andTEBAC (0.23 g, 1mmol) in 60 mLof benzene is stirred at reflux for 40 min. Then ethyl 2-aminoacetate (10 mmol) is added and stirring is continuedfor 10 min at reflux temperature. Theprecipitate is filtered off, and the filtrate is evaporated under reduced pressure. The carboxamide 8thus obtained is crystallized from MeOH to afford the pureproduct (yield 82%).

四、 Boc羧硫酸还原齐吡啶下面

Typicalprocedure:

To a stirred solution of N -protected amino acid 9(10 mmol), pyridine (0.5 ml) and Boc 2 O (3 g, 13 mmol) in an appropriate solvent (such asdioxane, DMF and CH 3 CN, 10-15 ml), ammonium hydrogencarbonate (1 g, 12.6 mmol) was added and the mixturewas stirred for 4-16 h. Ethyl acetatewas added and after washings with water and 5% H 2 SO 4 , thesolution was dried, the solvent was evaporated and the product was trituratedwith ether. In another variant the reactionmixture was diluted with water (30-40 ml), stirred until crystallization was completed,a residue was then collected by filtration, washed by water, dried and recrystallizedas necessary.

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