反应 #470359

ord-2297c9ba132c47f2a98b1e2367a9b2a2

反应方程式

CN1CCCC1
N-methylpyrrolidine
COCCl
Chloromethyl methyl ether
COC[N+]1(C)CCCC1.[Cl-]
desired product
COC[N+]1(C)CCCC1.[Cl-]
N-Methyl-N-Methoxymethylpyrrolidinium Chloride

溶剂

反应条件

温度
5°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度gradually heated to a higher temperature
  2. 2
    workup.STIRRINGstirred at room temperature for 10 hours
  3. 3
    其他the reaction
  4. 4
    过滤The reaction mixture was filtered
  5. 5
    洗涤the resulting solid product was washed with 150 g of toluene and 150 g of acetone
  6. 6
    其他The washed product was dried in a vacuum

实验过程

A 30.0 g quantity of N-methylpyrrolidine (reagent, product of Tokyo Kasei Co., Ltd.) was dissolved in 120 g of toluene, followed by replacement with nitrogen. Chloromethyl methyl ether (31.2 g, reagent, product of Tokyo Kasei Co., Ltd.) was added dropwise to the solution at 5° C. over a period of 1 hour. The mixture was stirred at 5° C. for 1 hour, then gradually heated to a higher temperature, and stirred at room temperature for 10 hours to complete the reaction. The reaction mixture was filtered, and the resulting solid product was washed with 150 g of toluene and 150 g of acetone. The washed product was dried in a vacuum to obtain 53.7 g of the desired product (white solid).

来源

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