Реакция #2050057

ord-ae3bb24121ea4854a6d21cbb4a62e16d

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted thrice with ethyl ether
  2. 2
    ДругоеThe two layers were separated
  3. 3
    КонцентрированиеThe aqueous layer was concentrated under reduced pressure

Методика

3-Methyl-3-prop-2-ynyloxymethyl-1-oxa-4-aza-spiro[4.5]decane (1.83 g) in an aqueous solution of HCl (6N) (2.73 ml) were refluxed for 1 hr. The reaction mixture was cooled down to room temperature, diluted with water and extracted thrice with ethyl ether. The two layers were separated. The aqueous layer was concentrated under reduced pressure to yield 2-amino-2-methyl-3-prop-2-ynyloxy-propan-1-ol hydrochloric salt (1.205 g) as a white beige solid which was used as such in Stage 3 described below. 1H NMR (DMSO) δ ppm: 8.02 (3H, s br); 5.47 (1H, s br); 4.21 (2H, s); 3.54-3.49 (5H, m); 1.15 (3H, s).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08415272B2uspto-grants-2013_04