反应 #470376

ord-f4819e69156d4d829fe4a5907091e3f1

反应方程式

CC(C)N1CCCC1
N-isopropylpyrrolidine
CCOCCl
chloromethyl ethyl ether
CCOC[N+]1(C(C)C)CCCC1.[Cl-]
desired product
CCOC[N+]1(C(C)C)CCCC1.[Cl-]
N-Ethoxymethyl-N-Isopropylpyrrolidinium Chloride

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was thereafter heated to a gradually elevated temperature
  2. 2
    其他whereby the reaction was terminated
  3. 3
    温度The reaction mixture was cooled to 5° C.
  4. 4
    过滤the resulting solids were filtered off in nitrogen
  5. 5
    洗涤The filter cake was washed with 200 ml of 2-butanone
  6. 6
    洗涤further washed with 200 ml of acetone
  7. 7
    其他dried in a vacuum

实验过程

A 40.09 g quantity of N-isopropylpyrrolidine was dissolved in 361 g of dehydrated 2-butanone (reagent, product of Wako Pure Chemical Ind. Ltd.), followed by replacement with nitrogen. To the solution was added dropwise 33.54 g of chloromethyl ethyl ether (reagent, product of Tokyo Kasei Co., Ltd. as purified by distillation) at 5° C. over a period of 0.5 hour. The mixture was thereafter heated to a gradually elevated temperature and stirred at room temperature for 10 hours, whereby the reaction was terminated. The reaction mixture was cooled to 5° C., and the resulting solids were filtered off in nitrogen. The filter cake was washed with 200 ml of 2-butanone, further washed with 200 ml of acetone and dried in a vacuum, giving 55.72 g of the desired product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08366956B2uspto-grants-2013_02