反应 #710532

ord-1a7fd1c2999b4aaa89245faa1cdccc57

反应条件

温度
25°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他solid was precipitated
  2. 2
    其他The solid was sufficiently precipitated
  3. 3
    workup.STIRRINGthe solution was stirred at 25° C. for 30 minutes
  4. 4
    其他Thereafter, the solid was separated by filtration under reduced pressure
  5. 5
    洗涤The solid was washed with methylene chloride (5 mL)
  6. 6
    其他drying

实验过程

Methanesulfonic acid (576 mg, 6 mmol) was added to a solution of (S)—N-(tert-butoxycarbonyl)nipecotic acid (1145 mg, 5 mmol) and methylene chloride (5 mL), and the mixture was stirred at 25° C. for 16 hours. Triethylamine (708 mg, 7 mmol) was added thereto, and then solid was precipitated. The solid was sufficiently precipitated, and then the solution was stirred at 25° C. for 30 minutes. Thereafter, the solid was separated by filtration under reduced pressure. The solid was washed with methylene chloride (5 mL), and then was subjected to vacuum drying. Thereby, the titled compound was produced as a white solid (238 mg, yield of 37%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09302980B2uspto-grants-2016_04