二甲胺亚甲基丙二腈

实验步骤: 投料: 取250ml单口瓶，加入甲醇钠，甲醇溶解，冰浴搅拌下加入盐酸丙脒，搅拌30min，过滤收集滤液，向滤液中分批加入二甲胺亚甲基丙二腈，RT搅拌过夜。\n监测: LCMS（18739-1-1）显示原料消失，主峰为产物峰（M+=149），将体系浓缩，除去部分甲醇，超声搅拌打浆，过滤干燥得米白色产物粗品6g。

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a slurry of 12.4 g. of 2-cyano-3-dimethylaminoacrolein in 50 ml. of water was added in small portions 13.6 g. of hydroxylamine-O-sulfonic acid (91% pure). The resulting clear solution was stirred for an additional 10 minutes, then cooled to 0° and adjusted to pH 6.0 by addition of approximately 26 ml. of 5N sodium hydroxide solution. The mixture was heated for 20 minutes in a water bath at 70°. A pH 3 was maintained over this period by dropwise addition of 5N sodium hydroxide solution. After cooling to room temperature, the mixture was extracted with 3 × 100 ml. of methylene chloride. The combined extracts were washed with 50 ml. of water, dried over magnesium sulfate, filtered and evaporated to dryness under reduced pressure. Thus, dimethylaminomethylenemalononitrile was obtained. After recrystallization from isopropanol, the material had a melting point of 93°-95°. cooled to 0° adjusted to pH 6.0 by addition of approximately 26 ml The mixture was heated for 20 minutes in a water bath at 70° the mixture was extracted with 3 × 100 ml The combined extracts were washed with 50 ml of water, dried over magnesium sulfate filtered evaporated to dryness under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a slurry of 12.4 g. of 2-cyano-3-dimethylaminoacrolein in 50 ml. of water was added in small portions 13.6 g. of hydroxylamine-0-sulfonic acid (91% pure). The resulting clear solution was stirred for an additional 10 minutes, then cooled to 0° and adjusted to pH 6.0 by addition of approximately 26 ml. of 5N sodium hydroxide solution. The mixture was heated for 20 minutes in a water bath at 70°. A pH 3 was maintained over this period by dropwise addition of 5N sodium hydroxide solution. After cooling to room temperature, the mixture was extracted with 3 × 100 ml. of methylene chloride. The combined extracts were washed with 50 ml. of water, dried over magnesium sulfate, filtered and evaporated to dryness under reduced pressure. Thus, dimethylaminomethylenemalononitrile was obtained. After recrystallization from isopropanol, the material had a melting point of 93°-95°. cooled to 0° adjusted to pH 6.0 by addition of approximately 26 ml The mixture was heated for 20 minutes in a water bath at 70° the mixture was extracted with 3 × 100 ml The combined extracts were washed with 50 ml of water, dried over magnesium sulfate filtered evaporated to dryness under reduced pressure