创新实验做不下去了，卡在中间，跪求大神解答TAT？ http:///us-5332735.html \ 这篇专利做了很多类似结构的化合物，主要是苯环上的取代基不同。用对羟基苯甲酸做成对羟基苯甲酰氯后与脯氨酸反应。 example 1: 4-hydroxy-1-(4,5-methylenedioxy-2-nitrobenzoyl)pyrrolidine-2-carboxylic acid (trans form) in a 2-liter three-necked round-bottomed flask equipped with 2 bromine funnels and a thermometer, a solution of 32 g (0.22 mole) of trans-4-hydroxyproline is cooled in an ice bath in 200 ml of water which is vigorously stirred. 22.8 g (0.1 mole) of 4,5-methylenedioxy-2-nitrobenzoyl chloride obtained in preparation 1 in solution in 150 ml of acetone are added dropwise, by means of the bromine funnel. simultaneously, a 40% solution of sodium hydroxide is also added dropwise so that the ph of the reaction mixture remains alkaline. the stirring is continued after the end of the addition for 20 minutes at room temperature. the acetone is removed under vacuum without exceeding 40.degree. c. the aqueous solution is then acidified and then left for 24 hours at room temperature. the crystals formed are spun, washed with water, dried and recrystallized in isopropanol. yield: 75% melting point: 230.degree. c. 查看更多
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