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A. (S)-Proline-N-carboxyanhydride. A dry, 3-L, three-necked flask, fitted with a mechanical stirrer, nitrogen inlet tube, 500-mL, pressure-equalized addition funnel and a Teflon-coated thermocouple probe, containing dry tetrahydrofuran (THF) (600 mL) is charged with (S)-proline (60.0 g, 0.521 mol) (Note 1). To the cooled (15–20°C) suspension is added phosgene (324 mL, 0.625 mol, 1.93 M in toluene), via a pressure-equalized addition funnel, over a 0.5–1.0 hr period maintaining a temperature of 15–20°C (Note 2). The reaction mixture is then aged for 0.5–0.75 hr at 30–40°C. The reaction mixture should become homogeneous as the proline reacts with the phosgene to afford the intermediate N-carbamoyl chloride. Once homogeneous, the reaction mixture is aged an additional 0.5 hr, then concentrated under reduced pressure (15–20°C, 1000 down to 50 mBar) to a volume of 80 mL (Note 3). Dry tetrahydrofuran (600 mL, KF < 50 μg/mL) is added to the mixture and it is cooled to 0–5°C. Dry triethylamine (72.6 mL, 0.521 mol, KF < 50 μg/mL) is added over 0.25 hr (Note 4). The mixture is aged for 0.5 hr at 0–5°C, then filtered through an enclosed, 2-L, medium-frit Schlenk funnel under an atmosphere of nitrogen (with careful exclusion of moisture). The triethylammonium hydrochloride cake is washed with dry tetrahydrofuran (3 × 105 mL, KF < 50 μg/mL). The filtrate and washes are combined and used as is in the next reaction (Note 5) and (Note 6). Caution! Benzene is generated in this reaction. Benzene is a known carcinogen. B. (S)-1,1-Diphenylprolinol. A 3-L, three-necked flask, fitted with a mechanical stirrer, nitrogen inlet tube, 1-L addition funnel and Teflon-coated thermocouple probe, is charged with phenylmagnesium chloride (0.80 L, 1.6 mol, 2.0 M in tetrahydrofuran) (Note 7) and cooled to −10°C (Note 8). To the suspension is added, with stirring, the tetrahydrofuran solution of (S)-proline-N-carboxyanhydride over a 1-hr period maintaining the temperature at −15° to −10°C (Note 9). After the addition is complete, the reaction mixture is aged for 3 hr at −15°C, then 1 hr at 0°C (Note 10). The reaction is quenched into a 5-L, mechanically-stirred flask containing 2 M aqueous sulfuric acid (1.05 L, 2.1 mol) (0°C) over a 0.5–1.0 hr period (Note 11). The reaction mixture is aged for 1 hr at 0–5°C, filtered, and the magnesium sulfate cake washed with tetrahydrofuran (3 × 500 mL) (Note 12). The filtrate and tetrahydrofuran washes are combined and concentrated (1 atm) to a volume of 1.0 L (Note 13). The mixture is cooled to 0°C, aged 1 hr, and then filtered. The cake is washed with water (5°C, 2 × 100 mL) and ethyl acetate (3 × 180 mL) (Note 14). The cake is dried under reduced pressure (40°C, 50 mBar) to yield 79–88 g (50–56% based on proline) of (S)-diphenylprolinol sulfate as a free-flowing white crystalline solid, mp 275–290°C (Note 15). A 3-L, three-necked flask, fitted with a mechanical stirrer, nitrogen inlet tube, and Teflon-coated thermocouple, is charged with (S)-diphenylprolinol sulfate (81.0 g, 0.268 mol), tetrahydrofuran (268 mL), and 2 M aqueous sodium hydroxide (268 mL). The mixture is stirred at 20–25°C until all the solid dissolves (0.5 hr) (Note 16). Toluene (1.1 L) is added and the mixture is aged 0.5 hr. The two-phase mixture is filtered through a medium frit sintered glass funnel and partitioned (Note 17). The upper layer is washed with water (130 mL) and the toluene is removed under reduced pressure to afford a light-tan colored oil that crystallizes upon standing at ambient temperature (Note 18). Recrystallization of the resulting light-tan crystals from heptane (ca. 2 mL of heptane per gram of prolinol) affords (S)-1,1-diphenylprolinol; [yield 64–68 g (94–99% yield based upon diphenylprolinol sulfate)] as white crystals, mp 76–78°C, >98% ee (Note 19),(Note 20)). Caution! Neat (10 M) borane-methyl sulfide is an air- and moisture-sensitive flammable liquid. Dimethyl sulfide has a noxious odor. All reactions should be conducted in an efficient fume hood. |
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：（S） - 脯氨酸的N-羧基。干燥3-L时，三口烧瓶，装有机械搅拌器，氮气入口管，500毫升，压力均衡除了漏斗和聚四氟乙烯涂层的热电偶探头含有干燥的四氢呋喃（THF）（600毫升），被控（S） - 脯氨酸（60.0克，0.521摩尔）（注1）。冷却（15-20℃）暂停加光气（324毫升，0.625摩尔，甲苯在1.93中号），通过压力扳平此外，漏斗超过0.5-1.0小时内保持温度15-20° ℃（注2）。 0.5-0.75小时的反应混合物，然后年龄在30-40°C。脯氨酸反应生成的光气负担中间的N-甲酰氯化反应混合物应成为均匀。一旦均匀，反应混合物岁增加0.5小时，然后集中到一个体积80毫升（注3）减压下（15-20℃，1000下降到50毫巴）。干燥的四氢呋喃（600毫升，氟化钾<50微克/毫升）的混合物冷却至0-5°C。干三乙胺（72.6毫升，0.521 mol时，氟化钾<50微克/毫升）添加了0.25小时（注4）。岁的混合物为0.5小时，在0-5℃，过滤，然后通过一个封闭的，2 - L，熔块中舒伦克氮气氛下的漏斗（小心排除水分）。三乙胺盐酸蛋糕洗净，用干燥的四氢呋喃（3×105毫升，KF <50微克/毫升）。滤液和洗涤相结合，并在接下来的反应（注5）和（注6）。 注意！在这个反应生成苯。苯是一种已知的致癌物质。 B.（）-1,1-Diphenylprolinol。苯基氯（0.80升，浓度为1.6 mol，2.0在四氢呋喃中号）（3 L时，三口烧瓶，装有机械搅拌器，氮气入口管，加入1-L的漏斗和聚四氟乙烯涂层的热电偶探头，被指控注7）和冷却到-10℃（注8）。暂停加搅拌，四氢呋喃溶液（S） - 脯氨酸N-羧基超过1小时期间保持温度在-15℃至-10℃（注9）。除了是完成后，反应混合物的年龄为3小时，于-15°C，然后在0°C（注10）1小时。到5-L机械搅拌瓶含有超过0.5-1.0小时内（注11）2米的硫酸水溶液（1.05升，2.1摩尔）（0℃）淬火反应。反应混合物1小时的年龄在0-5°，过滤，和硫酸镁蛋糕的四氢呋喃（3×500毫升）（注12）洗净。滤液和四氢呋喃清洗相结合，集中（1个大气压），容积为1.0升（注13）。将混合物冷却至0℃，现年1小时，然后过滤。蛋糕用清水洗净（5℃，2×100毫升）和乙酸乙酯（3×180毫升）（注14）。饼干下减少压力（40°，50毫巴）79-88克（50-56％的基础上脯氨酸）（S）diphenylprolinol硫酸产量作为一个自由流动的白色结晶固体，熔点275-290 ℃（注15）。 3 L时，三口烧瓶，装有机械搅拌器，氮气入口管，聚四氟乙烯涂层的热电偶，（S）diphenylprolinol硫酸（81.0克，0.268摩尔），四氢呋喃（268毫升），被指控2米的氢氧化钠溶液（268毫升）。将混合物搅拌在20-25°C，直到所有固体溶解（0.5小时）（注16）。甲苯（1.1 L），添加混合物岁0.5小时的。两相混合物通过中期熔块烧结玻璃漏斗过滤，并分区（注17）。上层洗涤水（130毫升）和甲苯，减少压力，负担轻棕褐色油，结晶后，在环境温度（注18）站在下删除。再结晶所产生的光谭庚（约2毫升每克的脯氨烷）给予晶体（S）-1,1-diphenylprolinol;产量64-68克（根据diphenylprolinol硫酸94-99％的产量）白色晶体，熔点76-78°C，> 98％ee的（注19），（注20））。 注意！整齐（10米）硼烷二甲硫醚是空气和水分敏感的易燃液体。二甲基硫醚，有臭味。所有的反应，应进行有效的通风柜。 你再看看，有什么不通顺的地方。我在帮你修改。 |
2楼2012-05-30 22:03:41
