1-Methyl-3-Pyrrolidinol CAS 13220-33-2 Purity >98.0% (GC)

Add 1,2,4-Butanetriol and glacial acetic acid to the reaction pot, stir and heat to about 100℃, add dry hydrogen chloride gas, and react at 90~110℃ for 30h, when a large amount of hydrogen chloride began to appear in the tail gas, the end point of the reaction was checked and the hydrogen chloride was stopped. After cooling, the material was discharged, washed with a saturated sodium carbonate solution, and subjected to distillation under reduced pressure, and 120 to 135℃. (12.6 to 13. 3kPa) fraction, I .e., 1,4-Dichloro-2-Butanol oily matter, yield 50%~60%.
Cyclization an aqueous solution of 1,4-Dichloro-2-Butanol and Methylamine was added to the cyclization pot, and heated to 120℃. Under closed heating, and the reaction was stirred for 10h. After cooling, solid sodium hydroxide was added, and the precipitated inorganic salt was filtered off. The oil layer was separated and subjected to vacuum distillation, and the fraction of 76-85℃. (2.1 kPa) was collected to be the finished product. Extraction of the aqueous layer with benzene also yields a portion of 1-Methyl-3-Pyrrolidinol. The yield was about 60%.
3. Key processes:
3.1 Substituted reaction process: control the reaction time and detect the reaction endpoint
3.2 Vacuum distillation process of 1,4-Dichloro-2-Butanol: control vacuum degree of vacuum distillation and fraction temperature
3.3 Cyclization reaction process: control reaction temperature and time
3.4 1-Methyl-3-Pyrrolidinol vacuum distillation process: control vacuum degree of vacuum distillation and fraction temperature
4. Quality control points:
Quality control point 1: 1,2,4-Butanetriol raw material quality standard
Quality control point 2: Central control quality standard for cyclization reaction
Quality control point 3: 1,4-Dichloro-2-Butanol intermediate quality standard
Quality control point 4: 1-Methyl-3-Pyrrolidinol finished product quality standard