Реакция #710532

ord-1a7fd1c2999b4aaa89245faa1cdccc57

Уравнение реакции

CS(=O)(=O)O
Methanesulfonic acid
CC(C)(C)OC(=O)N1CCC[C@H](C(=O)O)C1
(S)—N-(tert-butoxycarbonyl)nipecotic acid
CCN(CC)CC
Triethylamine
O=C(O)[C@H]1CCCNC1
titled compound
O=C(O)[C@H]1CCCNC1
(S)-nipecotic acid

Растворители

Условия реакции

Температура
25°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеsolid was precipitated
  2. 2
    ДругоеThe solid was sufficiently precipitated
  3. 3
    workup.STIRRINGthe solution was stirred at 25° C. for 30 minutes
  4. 4
    ДругоеThereafter, the solid was separated by filtration under reduced pressure
  5. 5
    ПромывкаThe solid was washed with methylene chloride (5 mL)
  6. 6
    Другоеdrying

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09302980B2uspto-grants-2016_04